CN104649691B - A kind of anti-thermal shock magnesia-spinel brick and preparation method thereof - Google Patents
A kind of anti-thermal shock magnesia-spinel brick and preparation method thereof Download PDFInfo
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Abstract
A kind of anti-thermal shock magnesia-spinel brick and preparation method thereof, this magnesia-spinel brick in use, is internally generated TiC and B4C non-oxidized substance phase, and MgFe2O4And Mg2TiO4Composite oxide solid solution phase, raw material is: fused magnesite granule and fine powder 70 ~ 85%, nano aluminum magnesia spinel powder body 3 ~ 10%,Micropowder 3 ~ 6%, aluminium powder 2 ~ 8%, nano-titanium oxide 0.5 ~ 10% and boric acid 2 ~ 5%, the addition containing carbon admixt be fused magnesite, nano aluminum magnesia spinel powder body,
Description
Technical field
The present invention relates to refining furnace magnesia-spinel brick, be specifically related to a kind of anti-thermal shock magnesia-spinel brick and preparation method thereof.
Background technology
Along with the progress of metallurgical industry, the continuous adjusting and optimizing of steel products structure, the demand of high-quality steel is increased by China further.Refining furnace steel-making is widelyd popularize as the secondary refining method that a kind of cost performance is the highest and is applied, and correspondingly, also refining furnace refractory material is proposed higher requirement.
At present, refining furnace refractory material is mainly based on magnesite-chrome brick, owing to this product contains chromium oxide, under high temperature, oxidizing atmosphere or alkali condition, and Cr therein3+Cr can be converted into6+, and Cr6+Soluble in water, additionally Cr2O3Can also exist with gas phase, contaminated air in air can be entered with flue gas in process of production, thus the environment such as water source, air, soil mass are produced extremely serious pollution, become superpower carcinogen, the harm that the healthy generation of the mankind is more serious.Prepare magnesite-chrome brick to need to use chrome ore raw material, and the chromium ore resource of China is poorer.Therefore people are devoted to the research and development work of RH refining furnace Chrome free refractories new product always.The Chinese patent that publication number is CN1715246 discloses a kind of RH vacuum furnace lining Chrome free refractories, and mainly magnesium zirconia refractory, zirconium oxide and the zircon of its use are expensive, cause production cost too high.Publication number is that the Chinese patent of CN102775156A discloses one and do not burn magnesia-spinel brick, and it is mainly corundum-spinel fire resistant materials, and this not burn the magnesia-spinel brick porosity higher, thermal shock resistance is poor.
Summary of the invention
It is an object of the invention to provide a kind of concrete relatively highly heatproof and shockproof stability, and in use, it is possible between magnesium oxide particle, form TiC and B4C non-oxidized substance phase, MgFe2O4And Mg2TiO4The magnesia-spinel brick of composite oxide solid solution phase, and the preparation method of this magnesia-spinel brick.
The technical scheme that the present invention adopts for achieving the above object is: a kind of anti-thermal shock magnesia-spinel brick, this magnesia-spinel brick is in use to be internally generated TiC and B after one can be applied to refining furnace4C non-oxidized substance phase, and MgFe2O4And Mg2TiO4The refractory brick of composite oxide solid solution phase, its by fused magnesite granule and fine powder, nano aluminum magnesia spinel powder body,Micropowder, aluminium powder, nano-titanium oxide, boric acid and form containing carbon admixt, by weight percentage, the addition of each raw material is followed successively by: fused magnesite granule and fine powder 70 ~ 85%, nano aluminum magnesia spinel powder body 3 ~ 10%,Micropowder 3 ~ 6%, aluminium powder 2 ~ 8%, nano-titanium oxide 0.5 ~ 10% and boric acid 2 ~ 5%, the addition containing carbon admixt be fused magnesite, nano aluminum magnesia spinel powder body,The 2.8 ~ 5.2% of micropowder, aluminium powder, nano-titanium oxide and boric acid gross weight.
In the present invention, for nano-titanium oxide, it is desirable to its granularity≤20nm, chemical composition requires TiO2≥99%；The granularity of aluminium powder is≤0.074mm, and its chemical composition requires Al >=99%.
In the present invention, the weight ratio of fused magnesite granule and fine powder is 58 ~ 69:10 ~ 15.Wherein, fused magnesite granule is made up of granule and the granule that particle diameter is 1 ~ 0.074mm of particle diameter to be the granule of 5 ~ 3mm, particle diameter be 3 ~ 1mm, 5 ~ 3mm, tri-kinds of granules of 3 ~ 1mm and 1 ~ 0.074mm weight ratio be 20～30:20～30:15～25；Granularity≤the 0.074mm of fused magnesite fine powder, its chemical constituent and mass percent thereof be: MgO >=98%, CaO≤1.0%, SiO2≤1.2%、Fe2O3≤1.0%；Igloss≤0.1%.
Nano aluminum magnesia spinel powder body in the present invention is sintered aluminium magnesia spinel and/or electric smelting aluminum-spinel, and the granularity of nano aluminum magnesia spinel powder body is 20 ~ 30nm, and its chemical constituent and mass percent thereof be: Al2O374～76%, MgO22～24%, Fe2O3≤ 0.5%, SiO2≤ 0.2%, surplus is impurity；Igloss≤0.1%.
In the present inventionMicropowder, granularity is 1 ~ 5 micron, and its chemical constituent and mass percent thereof be: Al2O3>=99%, Fe2O3≤ 0.2%, SiO2≤ 0.2%, surplus is impurity；Phase content >=90%, igloss≤0.5%.
In the present invention is one or more in thermosetting phenolic resin, thermoplastic phenolic resin or modified pitch resin containing carbon admixt.
The preparation method of a kind of anti-thermal shock magnesia-spinel brick, comprises the following steps: step one, according to above-mentioned percentage by weight: fused magnesite granule and fine powder 70 ~ 85%, nano aluminum magnesia spinel powder body 3 ~ 10%,Micropowder 3 ~ 6%, aluminium powder 2 ~ 8%, nano-titanium oxide 0.5 ~ 10% and boric acid 2 ~ 5%, the addition containing carbon admixt be fused magnesite, nano aluminum magnesia spinel powder body,The 2.8 ~ 5.2% of micropowder, aluminium powder, nano-titanium oxide and boric acid gross weight, the weight ratio of fused magnesite granule and fine powder is 58 ~ 69:10 ~ 15.Weigh fused magnesite fine powder, nano aluminum magnesia spinel powder body,Micropowder, aluminium powder, nano-titanium oxide and boric acid, and be sufficiently mixed, prepare premix, standby；
What step 2, step one weighed joins in fused magnesite granule containing carbon admixt, is sufficiently mixed stirring 5 ~ 10min, then adds the premix that step one prepares in this stirring container, be sufficiently mixed stirring 20 ~ 30min, prepares compound, standby；
Step 3, under 630T pressure condition, compound step 2 prepared adopts that semidry method is compressing makes adobe, by qualified adobe through natural drying 24h, and dried adobe processes at 400 ~ 500 DEG C 48 ~ 72h, prepared magnesia-spinel brick.Wherein, in this step, the press of the compressing employing of semidry method is any one in friction brickmaking machine, isostatic pressing machine or hydraulic press.
Aluminum-spinel is incorporated in magnesia-spinel brick with nano-powder form by the present invention, in order that reserve a part of spinelle nucleus in magnesia-spinel brick substrate, make fused magnesite and alumina powder based on this nucleus, in use there is spinel reaction, so that magnesia-spinel brick sinters as early as possible, produce to be similar to the crystal phase structure of magnesium aluminate spinel burnt product, to reach the purpose of anti-erosion, chipping resistance.
Beneficial effects of the present invention: containing nano-titanium oxide in the raw material of (1), the present invention, in the use procedure of magnesia-spinel brick, generates complicated MgFe2O4And Mg2TiO4Solid solution, oxide phase, particularly at iron content alkaline melt and CaFe2O4During slag action, following reaction is had to carry out: Fe+MgO+TiO2→MgFe2O4+Mg2TiO4, the MgFe of reaction generation2O4Solid solution covers on brick body surface or MgO granule, the corrosion resistance of reinforcing material and thermal shock resistance；The Mg generated2TiO4Solid solution, oxide mineral facies are present between MgO granule, can effectively prevent high-temperature fusant through the gap of the skeleton of resistance to material of MgO granule composition, improve the anti-scour property of magnesia-spinel brick.
(2), a kind of magnesia-spinel brick prepared by the present invention, raw material adds nano-titanium oxide, owing to surface activity and the specific surface area of nano-titanium oxide are bigger, the effect making the antioxidant of the metallic aluminium powder added obtains better performance, nano-titanium oxide, aluminium powder and the response speed containing carbon admixt three, much larger than aluminium powder and the response speed containing carbon admixt, significantly reduce Al4C3Residual in magnesia-spinel brick, significantly improve and given full play to the antioxidation caused by aluminium powder and high temperature potentiation, the TiC fusing point generated is high, in network structure, non-oxidizability scouring can be improved, compared with prior art, when using the aluminium powder of same amount to make antioxidant, add nano-titanium oxide and can improve the high-temperature oxidation resistance of magnesia-spinel brick；In the use procedure of this magnesia-spinel brick, at high temperature, boric acid reacts with the carbon introduced containing carbon admixt, generates the B combined with covalent bond4C non-oxidized substance phase, has the advantages that high-melting-point, high rigidity, wear-resisting, acid-alkali-corrosive-resisting and the coefficient of expansion are low.
(3) fused magnesite of nano aluminum magnesia spinel powder body, nano-titanium oxide, granule and fine-powdered that, in the raw material of the present invention, additional proportion is different, owing to nano-titanium oxide, nano aluminum magnesia spinel powder body do not mate with the thermal coefficient of expansion of fused magnesite, in thermal shock process, different stress fields can be produced, thus changing the microstructure of magnesia-spinel brick, improve the thermal shock resistance of magnesia-spinel brick；Meanwhile, nano-titanium oxide can reduce the overall thermal coefficient of expansion of magnesia-spinel brick, improves the consistency of brick body, thus improving the elevated temperature strength of magnesia-spinel brick.
(4) a kind of magnesia-spinel brick, prepared by the present invention, adopts chromium free raw material, will not produce Cr in producing and using6+, it is to avoid Cr6+Pollute, protect environment, it is to avoid Cr6+Healthy to the mankind produces harm；The preparation process of the present invention adopts exempts from high temperature firing process, and energy consumption is little, reduces production cost；A kind of magnesia-spinel brick prepared by the present invention, than existing magnesite-chrome brick, there is more excellent combination property demonstrating through capabilities of refractory materials test, its thermal shock residual strength conservation rate exceeds more than 30% than traditional Cr26 magnesia brick, high temperature break resistant intensity reaches more than 15MPa, cold crushing strength reaches more than 170MPa, long service life, security reliability is good.
Detailed description of the invention
A kind of anti-thermal shock magnesia-spinel brick, this magnesia-spinel brick is that one can be applied to refining furnace, and in use, magnesia-spinel brick is internally generated TiC and B4C non-oxidized substance phase, and MgFe2O4And Mg2TiO4Composite oxide solid solution phase, its by fused magnesite granule and fine powder, nano aluminum magnesia spinel powder body,Micropowder, aluminium powder, nano-titanium oxide, boric acid and form containing carbon admixt, by weight percentage, the addition of each raw material is followed successively by: fused magnesite granule and fine powder 70 ~ 85%, nano aluminum magnesia spinel powder body 3 ~ 10%,Micropowder 3 ~ 6%, aluminium powder 2 ~ 8%, nano-titanium oxide 0.5 ~ 10% and boric acid 2 ~ 5%, the addition containing carbon admixt be fused magnesite, nano aluminum magnesia spinel powder body,The 2.8 ~ 5.2% of micropowder, aluminium powder, nano-titanium oxide and boric acid gross weight.
Wherein, the weight ratio of fused magnesite granule and fine powder is 58 ~ 69:10 ~ 15；Fused magnesite granule is made up of granule and the granule that particle diameter is 1 ~ 0.074mm of particle diameter to be the granule of 5 ~ 3mm, particle diameter be 3 ~ 1mm, 5 ~ 3mm, tri-kinds of granules of 3 ~ 1mm and 1 ~ 0.074mm weight ratio be 20～30:20～30:15～25.
Wherein, the granularity≤0.074mm of fused magnesite fine powder, its chemical constituent and mass percent thereof be: MgO >=98%, CaO≤1.0%, SiO2≤1.2%、Fe2O3≤1.0%；Igloss≤0.1%.Nano aluminum magnesia spinel powder body is sintered aluminium magnesia spinel and/or electric smelting aluminum-spinel, and the granularity of nano aluminum magnesia spinel powder body is 20 ~ 30nm, and its chemical constituent and mass percent thereof be: Al2O374～76%, MgO22～24%, Fe2O3≤ 0.5%, SiO2≤ 0.2%, surplus is impurity；Igloss≤0.1%.
The present invention also provides for a kind of method producing above-mentioned magnesia-spinel brick, particularly as follows: first by fused magnesite fine powder, nano aluminum magnesia spinel powder body,Micropowder, aluminium powder, nano-titanium oxide and boric acid, by the percentage by weight proportioning of above-mentioned magnesia-spinel brick component, mix homogeneously, make premix；Being slowly added to containing carbon admixt, kneading 5 ~ 10min by disposable in 2min for fused magnesite granule again, be eventually adding kneading 20 ~ 30min discharging after all premixs, be then pressed into type, dry baking, kiln discharge is checked, and obtains described magnesia-spinel brick.Above-mentioned molding is to carry out on 630 tons and above tonnage presses；Above-mentioned dry baking need at 400 ~ 500 DEG C of heat treatment 48 ~ 72h.The press of compressing employing is any one in friction press, isostatic pressing machine or hydraulic press.
Embodiment 1 ~ 4, proportioning described according to the form below 1, by aforementioned production method, prepare the magnesia-spinel brick containing nano-titanium oxide.
Table 1 embodiment 1 ~ 4 proportioning raw materials table (percentage by weight)
Cr26(and Cr of embodiment 1 ~ 4 products obtained therefrom and the application of current refining furnace2O3Weight/mass percentage composition) magnesite-chrome brick, contrast test result is in Table 2, wherein, what embodiment 1 adopted is thermoplastic phenolic resin containing carbon admixt, what embodiment 2 adopted is modified pitch resin containing carbon admixt, what embodiment 3 adopted is thermosetting phenolic resin and modified pitch resin containing carbon admixt, and what embodiment 4 adopted is thermosetting phenolic resin, thermoplastic phenolic resin and modified pitch resin containing carbon admixt.
In table 2, (1), carry out apparent porosity, bulk density, cold crushing strength, high temperature break resistant intensity (1400 DEG C × 0.5h) according to country's compact refractory material standard of articles, burn after the detection of the project such as Linear change rate (1550 DEG C × 3h).(2), thermal shock resistance is to put into the thermal shock stove of 1100 DEG C with the batten of 160 × 40 × 40mm, insulation 20min, air-cooled 15min after taking-up, repeat this process 3 times repeatedly, residual strength after test thermal shock, using residual strength conservation rate measuring as thermal shock resistance quality.(3), the test of non-oxidizability be that goods are placed in electric furnace, heat in air atmosphere to 1550 DEG C, be incubated 3h, be cooled to room temperature tailing edge and be slit longitudinally into two halves, measure its practical decarburized depth.(4), slag corrosion resistance and permeability adopt Static crucible method, under 1650 DEG C of conditions, crucible sample is corroded with certain steel mill RH refinery cinder and the degree of depth of infiltration evaluates slag corrosion resistance and the permeability of product.
The product of table 2 embodiment 1 ~ 4 and the contrast of Cr26 magnesite-chrome brick performance indications
A kind of Chrome-free provided by the invention does not burn magnesia-spinel brick, and without chromium element and not carburetting, long service life, simple by production technology, good operational environment, energy consumption is little.The Chrome-free of the present invention does not burn magnesia-spinel brick and utilizes varigrained nano-titanium oxide mixed powder to improve the microstructure of magnesia-spinel brick, promotes that the metallic aluminium powder antioxidant used plays one's part to the full and improves the non-oxidizability of magnesia-spinel brick；Utilize nano-titanium oxide not mate with the thermal coefficient of expansion of magnesia, design different mismatch, improve the thermal shock resistance of magnesia-spinel brick；Utilize titanium oxide mixed powder so that between magnesium oxide particle, form the Mg of a kind of complexity2TiO4And MgFe2O4Oxide solid solution improves the resistance to slag corrosion of magnesia-spinel brick.MgFe2O4Dissolubility fluctuation in MgO is very big, when the temperature increases, and substantial amounts of MgFe2O4It is dissolved in lattice；When temperature reduces, then there is more weak anisotropic dendritic crystal and graininess inclusion enclave precipitating in the surface and cleavage crack of magnesia spinel granule, thus promoting the growth of its crystal and the sintering of goods.
By table 1 and table 2 it can be seen that the thermal shock residual strength conservation rate of magnesia-spinel brick, non-oxidizability, cold crushing strength and high temperature break resistant intensity that embodiment 1 ~ 4 prepares are superior to tradition Cr26 magnesite-chrome brick.This is owing to adding nano-titanium oxide in raw material, introduces carbon simple substance containing carbon admixt, and raw material carries out reaction: 4Al+3C+3TiO as follows2=2Al2O3+ 3TiC, owing to nano-titanium oxide surface activity is big, specific surface area is big so that this reaction is more easy to and carries out, and significantly reduces aluminum and the Al of carbon simple substance reaction generation4C3Residual in brick body, hence it is evident that improve and given full play to antioxidation and high temperature potentiation that metallic aluminium powder is risen.The facilitation of the titanium oxide of smaller particle size, the effect making the antioxidant of the metallic aluminium powder added obtains better performance, therefore, when using the metallic aluminium powder of less content to make antioxidant, add nano-titanium oxide and can improve the high-temperature oxidation resistance of magnesia-spinel brick.And, raw material adds the nano-titanium oxide of different content and ratio, owing to nano-titanium oxide does not mate with the thermal coefficient of expansion of magnesia, in thermal shock process, different stress fields being produced, thus changing the microstructure of magnesia-spinel brick, improving the thermal shock resistance of magnesia-spinel brick.
Listed above is only specific embodiments of the invention, it is clear that the invention is not restricted to above example, has many similar changes therewith.If all deformation that those skilled in the art directly derives from present disclosure or associates, protection scope of the present invention all should be belonged to.
Claims (7)
1. an anti-thermal shock magnesia-spinel brick, it is characterised in that: this magnesia-spinel brick is in use to be internally generated TiC and B after one can be applied to refining furnace4C non-oxidized substance phase, and MgFe2O4And Mg2TiO4The refractory brick of composite oxide solid solution phase, it is by fused magnesite granule and fine powder, nano aluminum magnesia spinel powder body, α-Al2O3Micropowder, aluminium powder, nano-titanium oxide, boric acid and containing carbon admixt form, by weight percentage, the addition of each raw material is followed successively by: fused magnesite granule and fine powder 70 ~ 85%, nano aluminum magnesia spinel powder body 3 ~ 10%, α-Al2O3Micropowder 3 ~ 6%, aluminium powder 2 ~ 8%, nano-titanium oxide 0.5 ~ 10% and boric acid 2 ~ 5%, the addition containing carbon admixt is fused magnesite, nano aluminum magnesia spinel powder body, α-Al2O3The 2.8 ~ 5.2% of micropowder, aluminium powder, nano-titanium oxide and boric acid gross weight, described fused magnesite granule is made up of granule and the granule that particle diameter is 1 ~ 0.074mm of particle diameter to be the granule of 5 ~ 3mm, particle diameter be 3 ~ 1mm, 5 ~ 3mm, tri-kinds of granules of 3 ~ 1mm and 1 ~ 0.074mm weight ratio be 20～30:20～30:15～25, granularity≤the 0.074mm of described fused magnesite fine powder, the granularity of described nano aluminum magnesia spinel powder body is 20 ~ 30nm.
2. a kind of anti-thermal shock magnesia-spinel brick according to claim 1, it is characterised in that: the weight ratio of described fused magnesite granule and fine powder is 58 ~ 69:10 ~ 15.
3. a kind of anti-thermal shock magnesia-spinel brick according to claim 1 and 2, it is characterised in that: chemical constituent and the mass percent thereof of described fused magnesite fine powder be: MgO >=98%, CaO≤1.0%, SiO2≤1.2%、Fe2O3≤1.0%；Igloss≤0.1%.
4. a kind of anti-thermal shock magnesia-spinel brick according to claim 1, it is characterized in that: described nano aluminum magnesia spinel powder body is sintered aluminium magnesia spinel and/or electric smelting aluminum-spinel, chemical constituent and the mass percent thereof of nano aluminum magnesia spinel powder body be: Al2O374～76%, MgO22～24%, Fe2O3≤ 0.5%, SiO2≤ 0.2%, surplus is impurity；Igloss≤0.1%.
5. a kind of anti-thermal shock magnesia-spinel brick according to claim 1, it is characterised in that: described is one or more in thermosetting phenolic resin, thermoplastic phenolic resin or modified pitch resin containing carbon admixt.
6. the preparation method of an anti-thermal shock magnesia-spinel brick as claimed in claim 2, it is characterised in that comprise the following steps:
Step one, percentage by weight according to described raw material, weigh fused magnesite fine powder, nano aluminum magnesia spinel powder body, α-Al successively2O3Micropowder, aluminium powder, nano-titanium oxide, boric acid and containing carbon admixt, then by fused magnesite fine powder, nano aluminum magnesia spinel powder body, α-Al2O3Micropowder, aluminium powder, nano-titanium oxide and boric acid are sufficiently mixed, and prepare premix, standby；
Step 2, percentage by weight according to described raw material, weigh fused magnesite granule, and step one weighed join in fused magnesite granule containing carbon admixt, it is sufficiently mixed stirring 5 ~ 10min, the premix that step one prepares is added again in this stirring container, it is sufficiently mixed stirring 20 ~ 30min, prepares compound, standby；
Step 3, under 630T pressure condition, compound step 2 prepared adopts that semidry method is compressing makes adobe, by qualified adobe through natural drying 24h, and dried adobe processes at 400 ~ 500 DEG C 48 ~ 72h, prepared magnesia-spinel brick.
7. the preparation method of anti-thermal shock magnesia-spinel brick according to claim 6, it is characterised in that: in step 3, the press of the compressing employing of semidry method is any one in friction brickmaking machine, isostatic pressing machine or hydraulic press.
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| CN105585322A (en) * | 2015-12-21 | 2016-05-18 | 洛阳利尔耐火材料有限公司 | Slag-corrosion-resistant magnesite-spinel brick and preparation method thereof |
| CN107663097B (en) * | 2017-09-28 | 2020-10-16 | 辽宁中镁高温材料有限公司 | High-performance compact composite titanium spinel brick and manufacturing method thereof |
| CN108191439B (en) * | 2018-02-28 | 2021-04-27 | 攀钢冶金材料有限责任公司 | Refractory brick for blast furnace slag high-temperature carbonization electric furnace and preparation method thereof |
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| CN101613207A (en) * | 2008-12-31 | 2009-12-30 | 北京利尔高温材料股份有限公司 | A kind of low-carbon corundum spinelle brick for refined steel ladles and preparation method thereof |
| CN101973771A (en) * | 2010-09-29 | 2011-02-16 | 淄博市鲁中耐火材料有限公司 | Ferrous aluminum and magnesium system refractory raw material and preparation method thereof |
| CN102775156A (en) * | 2011-05-13 | 2012-11-14 | 宝山钢铁股份有限公司 | Unburned magnesium-aluminum spinel brick |
| CN102936142A (en) * | 2012-11-06 | 2013-02-20 | 河北联合大学 | Magnesia carbon brick added with manganese dioxide and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101613207A (en) * | 2008-12-31 | 2009-12-30 | 北京利尔高温材料股份有限公司 | A kind of low-carbon corundum spinelle brick for refined steel ladles and preparation method thereof |
| CN101973771A (en) * | 2010-09-29 | 2011-02-16 | 淄博市鲁中耐火材料有限公司 | Ferrous aluminum and magnesium system refractory raw material and preparation method thereof |
| CN102775156A (en) * | 2011-05-13 | 2012-11-14 | 宝山钢铁股份有限公司 | Unburned magnesium-aluminum spinel brick |
| CN102936142A (en) * | 2012-11-06 | 2013-02-20 | 河北联合大学 | Magnesia carbon brick added with manganese dioxide and preparation method thereof |
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