CN105753487B - Improve the composite granule and preparation method thereof of carbon containing refractory scour resistance - Google Patents

Improve the composite granule and preparation method thereof of carbon containing refractory scour resistance Download PDF

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CN105753487B
CN105753487B CN201610114063.9A CN201610114063A CN105753487B CN 105753487 B CN105753487 B CN 105753487B CN 201610114063 A CN201610114063 A CN 201610114063A CN 105753487 B CN105753487 B CN 105753487B
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composite granule
zirconium
mesh
zirconia
zirconium carbide
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CN105753487A (en
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钱凡
李红霞
刘国齐
杨文刚
于建宾
马谓奎
王刚
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
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    • 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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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • 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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Abstract

The invention belongs to carbon containing refractory preparing technical fields, relate generally to a kind of composite granule and preparation method thereof improving carbon containing refractory scour resistance.A kind of composite granule of the anti-scour resistance of raising carbon containing refractory proposed is combined by zirconium carbide particle and nanoscale zirconia；The mass ratio of nanoscale zirconia described in composite granule and zirconium carbide particle is 0.5:1~1:0.5；The granularity of the zirconium carbide particle is the mesh of 200 mesh~400, is located at the center of composite granule；The nanoscale zirconia is the partially stabilized zirconia that granularity is less than 30nm；The nanoscale zirconia is evenly dispersed and is wrapped in the outer surface of zirconium zirconium particle；The granularity of the composite granule is more than 150 mesh, and is less than 80 mesh.The present invention ensures that zirconium oxide is strong in the surface adhesion force of zirconium carbide, while the broken suitable granularity of acquisition is carried out after drying, and finally obtains nanoscale zirconia and coat zirconium carbide composite granule.

Description

Improve the composite granule and preparation method thereof of carbon containing refractory scour resistance
Technical field
The invention belongs to carbon containing refractory preparing technical fields, relate generally to a kind of raising carbon containing refractory antiscour Composite granule of performance and preparation method thereof.
Background technology
Carbon containing refractory is widely used in continuous casting industrial flow, wherein the application with continuous-casting three-main-product is the most universal, However carbon containing refractory itself carbon network under molten steel atmosphere（In conjunction with carbon and graphite）Structure is caused to be dredged because dissolving or aoxidizing Pine, it is difficult to resist molten steel wash away and the infiltration of slag corrode, antioxidant is largely introduced into carbon containing refractory thus In, the substances such as boron, silicon, such as patent ZL200810011972.5 boracic antioxidants are generally contained in current anti-oxidizing agent Its oxidation product be with the presence of liquid phase, the oxidation product antiscour containing siliceous antioxidant of ZL200910066119.8 descriptions and Erosion-resisting characteristics is poor.
Zirconium carbide is a kind of substance relatively common in carbide material, with carbonaceous material institute with many excellent spies Property, the anti-oxidizing agent of carbon containing refractory is may be used as, starts oxidizing temperature in air and is less than resin oxidation of coal temperature Degree, oxidation product ZrO2High-temperature behavior is good, however under aerobic atmosphere, it, should with the raising ZrC particles meeting vigorous oxidation of temperature Process can have volume expansion and also result in particle fracture so that loose decarburized layer becomes further fragile, reduces its anti-steel Liquid wash away and erosiveness.
Existing zirconium carbide is as antioxidant its main function can be prior to oxidation of coal, however due to its oxidation reaction companion It with bulk effect, is easy to cause that article construction is loose, weakens the erosion resistibility of product.
Invention content
In order to overcome above-mentioned deficiency, the purpose of the present invention is to propose to a kind of raising anti-scour resistances of carbon containing refractory Composite granule and preparation method thereof.
The present invention is to complete foregoing invention task to adopt the following technical scheme that：
A kind of composite granule improving the anti-scour resistance of carbon containing refractory, the composite granule is by zirconium carbide particle It is combined with nanoscale zirconia；The mass ratio of nanoscale zirconia described in composite granule and zirconium carbide particle is 0.5:1 ~1:0.5；The granularity of the zirconium carbide particle is the mesh of 200 mesh~400, is located at the center of composite granule；The nanoscale oxygen It is the partially stabilized zirconia that granularity is less than 30nm to change zirconium；The nanoscale zirconia is evenly dispersed and is wrapped in zirconium zirconium The outer surface of grain；The granularity of the composite granule is more than 150 mesh, and is less than 80 mesh.
The partially stabilized zirconia is stable calcium oxide zirconium oxide or stabilized magnesium hydroxide zirconium oxide or stabilized with yttrium oxide Zirconium oxide.
A kind of preparation method for the composite granule improving the anti-scour resistance of carbon containing refractory, the preparation method are adopted It is prepared with Gel-casting process, the specific steps are：Organic monomer, crosslinking agent are first put into dissolving in the beaker for fill solvent to obtain Premixed liquid, and premixed liquid is poured into ball grinder；Then by nanoscale zirconia and zirconium carbide particle according to 0.5:1~1:0.5 Mass ratio be added in ball grinder, and it is mill ball that zirconia ball, which is added, in ball grinder, and slurry is made after 20 hours in ball milling Material；Initiator and catalyst is added into slurry respectively again；It is injected into molding die inner gel curing molding；Mould is sloughed after solidification Tool obtains green body, and green body is put into climatic chamber, keeps dry under 20~30 DEG C of temperature, 80~90% environment of humidity, so It by green body and is crushed afterwards, obtains granularity and be more than 150 mesh, the nano zircite for being less than 80 mesh wraps up zirconium carbide composite granule.
Organic monomer, crosslinking agent, initiator, the catalyst of the Gel-casting process selection are respectively acrylic amine, Asia Bisacrylamide, ammonium persulfate, tetramethylethylenediamine；Solvent is water.
The total amount of the nanoscale zirconia and zirconium carbide particle accounts for the 60%~85% of slurry gross mass, solvent in slurry, Organic monomer, crosslinking agent mass ratio be 100：15~20：5~3；Initiator, catalyst charge are organic monomer quality 1%~3%, 0.5%~2%.
The carbonaceous material is aluminum-carbon refractory material or magnesia-carbon refractory material or aluminum-spinel carbon refractory.
It is added to account in preparing carbon containing refractory mixing process and prepares carbon containing refractory solid material weight 2 ~ 6% Composite granule, the introducing of composite granule can improve the scour resistance of above-mentioned carbon containing refractory.
A kind of composite granule and preparation method thereof improving the anti-scour resistance of carbon containing refractory proposed by the present invention, receives Meter level zirconium oxide can preferably be coated on zirconium carbide surface, because of the grain of the nanoscale zirconia introduced surmised compared with zirconium carbide Degree is thin, and surface area is big, by controlling ratio between the two, while by Gel-casting process, ensure that nanoscale zirconia Powder is evenly dispersed and wraps up zirconium zirconium particle, while making monomer polymerization and crosslinking, structure using the effect of catalyst and initiator At three-dimensional network, ceramic suspension body is enabled to solidify in situ, ensure that green body during follow-up broken and introducing carbon containing refractory, This package effect continues；Nano zircite dispersion is set fully to be coated on zirconium carbide surface and avoid the reunion of itself, it should Technique ensures that zirconium oxide is strong in the surface adhesion force of zirconium carbide, while the broken suitable granularity of acquisition is carried out after drying, and final It obtains nanoscale zirconia and coats zirconium carbide composite granule；The activity of the nanoscale zirconia is high, and the energy of oxidation of zirconium carbide Power is strong, and after the powder is introduced into carbonaceous material composition, in application process after forming decarburized layer, carbon network disappears product It loses, under molten steel temperature, the nano zircite（Stabilized with yttrium oxide, 1400 DEG C or so of sintering temperature, elevated temperature strength are high）It can be certainly Body is sintered, and forms zirconium oxide combination network, erosion resistibility is strong, while containing ZrC in the composite granule, can play anti-oxidant The effect of agent is without generating liquid phase, while volume has certain expansion after its oxidation, avoids sintering and causes larger volume It shrinks.
Specific implementation mode
Embodiment 1
Nano zircite grade coats the preparation of zirconium carbide composite granule：
1）Prepare slurry：166.5 grams of acrylamides, 33.3 grams of methylene-bisacrylamides are put into and fill 1110 grams of water Dissolving obtains premixed liquid in beaker, pours into ball grinder；666 grams of zirconium carbides are weighed respectively（200 mesh）, 1332 grams of nano zircites （Granularity is less than 30nm, and yttrium oxide part is stablized）Zirconium oxide, using zirconia ball as mill ball, slurry is made after 20 hours in ball milling；
2）Molding and drying：Again respectively to step 1）Slurry in 1.7 grams of initiator ammonium persulfates and 0.8 gram be added urge Agent tetramethylethylenediamine；It is injected into molding die, gel solidification is molded under 30 DEG C, 80%RH humidity；It is sloughed after solidification Mold obtains green body, and green body is put into climatic chamber, keeps dry under 25 DEG C of temperature, 90% environment of humidity, then by base Body is simultaneously crushed, and is obtained granularity and is more than 150 mesh, and the nano zircite for being less than 80 mesh wraps up zirconium carbide composite granule；
Application of the cladding zirconium carbide composite granule containing nano zircite as precursor in aluminum-carbon refractory material：Aluminium oxide It is primary raw material with graphite, wherein aluminium oxide accounts for the 90% of weight, and graphite accounts for the 10% of weight, and successively adds packet containing nano zircite Zirconium carbide composite granule, solid resin powder, liquid resin, alcohol, Wu Tuo are covered, weight is put account for aluminium oxide and graphite gross weight respectively 2%, 2%, 8%, 3.5%, the 0.6% of amount.Be kneaded through high speed mixer, control blank fugitive constituent 1.2%, in 120MPa isostatic presseds at Type is finally heat-treated in nitrogen atmosphere protection treatment furnace, N2Content is more than 99.99vol%, and 1000 are warming up to 1 DEG C/min DEG C, keep the temperature 300min.The normal elevated temperature strength of aluminum-carbon refractory material distinguishes 14.7MPa and 12.5MPa after heat treatment.1100 DEG C of water coolings Residual strength is 10.1MPa after thermal shock 4 times.
Case study on implementation 2
Nano zircite coats zirconium carbide composite granule and prepares：1）Prepare slurry：By 220 grams of acrylamides, 55.0 grams of Asias Bisacrylamide, which is put into fill to dissolve in 1100 grams of water beakers, obtains premixed liquid, pours into ball grinder；2597 are weighed respectively Gram carbonization zirconium powder（400 mesh）, 5195 grams of nano zircites（Granularity is less than 30nm, and magnesia part is stablized）, with zirconia ball be Slurry is made after 20 hours in mill ball, ball milling.2）Molding and drying：6.6 grams of initiations are added into the slurry of step 1 respectively again Agent ammonium persulfate and 4.4 grams of catalyst tetramethylethylenediamines.It is injected into molding die, the gel under 30 DEG C, 80%RH humidity Curing molding.Mold is sloughed after solidification and obtains green body, green body is put into climatic chamber, keeps 25 DEG C of temperature, humidity 90% It is dry under environment, it then by green body and is crushed, obtains granularity and be more than 150 mesh, the nano zircite for being less than 50 mesh wraps up zirconium carbide Composite granule.
Application of the cladding zirconium carbide composite granule containing nano zircite as precursor in magnesia-carbon refractory material：Aluminium oxide It is primary raw material with graphite, wherein magnesia accounts for the 94% of weight, and graphite accounts for the 6% of weight, and is successively added and contains nano zircite Coat zirconium carbide composite granule, solid resin powder, liquid resin, alcohol, Wu Tuo, weight is put respectively accounts for aluminium oxide and graphite is total 4%, 4%, 2%, 3.5%, the 0.7% of weight.Be kneaded through high speed mixer, control blank fugitive constituent 1.1%, in 120MPa isostatic presseds at Type is finally heat-treated in nitrogen atmosphere protection treatment furnace, N2Content is more than 99.99vol%, and 1200 are warming up to 1 DEG C/min DEG C, keep the temperature 300min.The normal elevated temperature strength of magnesia-carbon refractory material distinguishes 16.5MPa and 12.3MPa.1100 DEG C of water cooling thermal shocks 4 times Residual strength is 8.2MPa afterwards.
Case study on implementation 3
Nano zircite coats zirconium carbide composite granule and prepares：1）Prepare slurry：By 195 grams of acrylamides, 43.0 grams of Asias Bisacrylamide, which is put into fill to dissolve in 1084 grams of water beakers, obtains premixed liquid, pours into ball grinder；1542 are weighed respectively Gram zirconium carbide（325 mesh）, 1542 grams of nano zircites（Granularity is less than 30nm, and calcium oxide part is stablized）, with alumina balls be grind Slurry is made after 20 hours in abrading-ball, ball milling.2）Molding and drying：3.9 grams of initiators are added into the slurry of step 1 respectively again Ammonium persulfate and 2.0 grams of catalyst tetramethylethylenediamines.It is injected into molding die, gel is solid under 30 DEG C, 80%RH humidity Chemical conversion type.Mold is sloughed after solidification and obtains green body, green body is put into climatic chamber, keeps 25 DEG C of temperature, 90% ring of humidity It is dry under border, it then by green body and is crushed, obtains granularity and be more than 150 mesh, the nano zircite cladding zirconium carbide for being less than 50 mesh is multiple Close powder.
The answering in aluminum-spinel carbon refractory as precursor of the cladding zirconium carbide composite granule containing nano zircite With：Aluminum-spinel and graphite are primary raw material, and wherein spinelle accounts for the 92% of weight, and graphite accounts for the 8% of weight, and is successively added Containing nano zircite cladding zirconium carbide composite granule, solid resin powder, furfural, Wu Tuo, weight is put account for aluminum-spinel respectively With 6%, 6.2%, 6.9%, the 0.5% of graphite total weight.It is kneaded through high speed mixer, control blank fugitive constituent 2.7%, in 40MPa etc. Hydrostatic profile is finally heat-treated in atmosphere protection treatment furnace, N2Content is more than 99.99vol%, is warming up to 1 DEG C/min 1200 DEG C, keep the temperature 300min.The normal elevated temperature strength of spinelle carbon refractory is respectively 18.5MPa and 15.3MPa.1100 DEG C of water It is cold and hot shake 4 times after residual strength be 7.1MPa.

Claims (4)

1. a kind of preparation method for the composite granule improving the anti-scour resistance of carbon containing refractory, it is characterised in that：Described Composite granule is combined by zirconium carbide particle and nanoscale zirconia；Nanoscale zirconia described in composite granule and zirconium carbide The mass ratio of particle is 0.5:1~1:0.5；The granularity of the zirconium carbide particle is the mesh of 200 mesh~400, is located at composite granule Center；The nanoscale zirconia is the partially stabilized zirconia that granularity is less than 30nm；The nanoscale zirconia is uniform Disperse and be wrapped in the outer surface of zirconium zirconium particle；The granularity of the composite granule is more than 150 mesh, and is less than 80 mesh, described Preparation method is prepared using Gel-casting process, the specific steps are：Organic monomer, crosslinking agent are first put into the beaker for filling solvent Middle dissolving obtains premixed liquid, and premixed liquid is poured into ball grinder；Then by nanoscale zirconia and zirconium carbide particle according to 0.5:1~1:0.5 mass ratio is added in ball grinder, and it is mill ball that zirconia ball, which is added, in ball grinder, and ball milling 20 is small Slurry is made in Shi Hou；Initiator and catalyst is added into slurry respectively again；It is injected into molding die inner gel curing molding； Mold is sloughed after solidification and obtains green body, green body is put into climatic chamber, keeps 20~30 DEG C of temperature, 80~90% ring of humidity It is dry under border, then green body is crushed, granularity is obtained and is more than 150 mesh, the nano zircite package zirconium carbide for being less than 80 mesh is compound Powder；The total amount of the nanoscale zirconia and zirconium carbide particle accounts for the 60% ~ 85% of slurry gross mass, solvent in slurry, organic Monomer, crosslinking agent mass ratio be 100：15~20：5~3；Initiator, catalyst charge be organic monomer quality 1% ~ 3%, 0.5%~2%。
2. a kind of preparation method of composite granule improving the anti-scour resistance of carbon containing refractory as described in claim 1, It is characterized in that：The partially stabilized zirconia is that stable calcium oxide zirconium oxide or stabilized magnesium hydroxide zirconium oxide or yttrium oxide are steady Determine zirconium oxide.
3. a kind of preparation method of composite granule improving the anti-scour resistance of carbon containing refractory as described in claim 1, It is characterized in that：Organic monomer that the Gel-casting process is selected, crosslinking agent, initiator, catalyst be respectively acrylic amine, Methylene-bisacrylamide, ammonium persulfate, tetramethylethylenediamine；Solvent is water.
4. a kind of preparation method of composite granule improving the anti-scour resistance of carbon containing refractory as described in claim 1, It is characterized in that：The carbonaceous material is aluminum-carbon refractory material or magnesia-carbon refractory material or aluminum-spinel carbon refractory.
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CN107235732B (en) * 2017-04-21 2020-07-31 宜兴市丁山耐火器材有限公司 Mullite coated refractory material
CN107266094A (en) * 2017-07-19 2017-10-20 合肥铭佑高温技术有限公司 A kind of preparation method of refractory material for casting technique
CN107399959B (en) * 2017-08-22 2020-10-16 东北大学 Preparation method for reinforcing aluminum oxide-magnesium oxide-calcium oxide composite material by using nano oxide
CN108358650A (en) * 2018-03-02 2018-08-03 合肥铭佑高温技术有限公司 A kind of preparation method of high-temperature refractory
CN108706983A (en) * 2018-07-11 2018-10-26 合肥铭佑高温技术有限公司 A kind of high strength refractory material and preparation method thereof
CN111646506B (en) * 2020-07-21 2023-01-03 宁德三祥纳米新材料有限公司 Method for preparing nano zirconium oxide by internal gel method
CN116410008A (en) * 2023-04-24 2023-07-11 鞍山市和丰耐火材料有限公司 Long-service-life low-carbon magnesia carbon brick and preparation method thereof

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