CN102627463B - Aluminum-spinel-corundum composite refractory material and preparation method as well as application thereof - Google Patents
Aluminum-spinel-corundum composite refractory material and preparation method as well as application thereof Download PDFInfo
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Abstract
The invention belongs to the field of refractory materials, and discloses an aluminum-spinel-corundum composite refractory material and a preparation method as well as application thereof. The aluminum-spinel-corundum composite refractory material comprises raw materials consisting of one or more of the following materials in percentage by weight and an inorganic binding agent: 1-15 percent of metal aluminum powder, 5-25 percent of magnesium-aluminum spinel and 73-90 percent of white corundum or plate-like corundum, wherein the amount of the inorganic binding agent is 1.5-3 percent of the total weight of the raw materials. The aluminum-spinel-corundum composite refractory material can be applied to preparing an RH (Ruhrstahl-Heraeus) refining furnace lining. According to the invention, the corundum, the spinel and the metal aluminum are used as raw materials; chromium pollution and carbon pollution are not introduced in a secondary refining process; the melting point of added metal aluminum is low; the aim of enhancing the corrosion resistance of the material is fulfilled by introducing a soft transition plastic phase matrix into the material and controlling the content of the transition plastic phase matrix; high-temperature firing is not required; the energy consumption is reduced; the cost is saved; the production period is shortened; and the quality and the life of a product are improved.
Description
Technical field
The invention belongs to fire resisting material field, relate to a kind of alumina-spinelle-corundum composite refractory material and its preparation method and application.
Background technology
The features such as it is high that RH refining furnace has efficiency, and facility investment is few, and metallurgical effect is good, are widely used in the smelting of high-quality Clean Steel and ultra low-carbon steel both at home and abroad.But RH refining is always not high with the work-ing life of refractory materials lining, takies no small share in production cost.Major cause has: 1. external refining temperature is high; 2. slag penetration enters refractory materials and reacts with it and cause thermal spalling and structure spalling; 3. be blown into O
2or Ar gas, or induction stirring, make molten steel, slag generation vigorous agitation, thereby cause refractory materials to be subject to strongly washing away of molten steel, refractory lining surface is constantly updated, thus the carrying out that has aggravated chemical erosion and dissolution process.
Traditional magnesia chrome brick is all outstanding in aspect performances such as thermal shock resistance and slag resistance, due to Cr
2o
3, can improve resistance to fouling and the heat-shock resistance of magnesite refractory, reduce thermal conductivity, therefore, in Steel industry, be widely used in secondary fine furnace, be widely used inner lining material in the most of steel mills of present China external refining equipment.But, containing Cr
2o
3, refractory materials at oxidizing atmosphere or a large amount of basic oxide as K
2o, Na
2when O, CaO etc. exist, its trivalent chromium (Cr at a certain temperature
3+) can change sexavalent chrome (Cr into
6+).Sexavalent chrome is a kind of material that human health is had to serious harm.Due to hexavalent chromium compound water soluble, also can gas phase form exist, therefore sexavalent chrome can enter in atmosphere by flue gas, also can be water-soluble and polluted source.Therefore, some advanced countries have worked out strict limitation standard to sexavalent chrome.Further strengthen the adaptability research of refractory materials to pyrotic smelting technique, focus on the impact research of refractory materials on Clean Steel quality, realize energy-saving and environmental protection, the high efficiency of refractory materials, will represent the researchdevelopment direction of refractory materials of new generation.
In magnesia, add graphite, make magnesia carbon brick, overcome the heat-shock resistance of MgO brick poor with the slag shortcoming that easily infiltration is very dark, structure spalling is serious, so magnesia carbon brick and magnesium calcium carbon (MgO-CaO-C) brick can be made lining brick for the refining furnace of some low-carbon (LC) Clean Steels of refining and carbon element steel alloy.Because carbon solubleness in iron is large, and carbon is soluble in molten steel, so refining ultra low-carbon steel should avoid molten steel to contact with carbon containing refractory during as Ultra-low carbon sheet steel.Therefore, traditional technology magnesia carbon brick can produce carburetting to ultra low-carbon steel.Identical with magnesia chrome brick, there is the high energy consumption of production and the graphite of a large amount of preciousnesses, the problems such as waste of chromium ore resource, thereby restricting, develop.Address these problems and need the progress of refractory materials production technology, develop novel material, replace production and the use containing chromium material completely.
K Shimizu etc. has developed MgO-Y
2o
3refractory materials, and built in RH vacuum chamber bottom, draw MgO-Y
2o
3brick with directly in conjunction with identical result of magnesia chrome brick life-span.Due to Y
2o
3be rare elements oxide compound, more expensive; If add-on is many, the popularization of this kind of brick will be met difficulty.
For improving the slag resistance of RH inner lining body based material, occurred in Al2O3-MgO matter mould material, introducing zirconium white or zircon micropowder or introducing a small amount of Fe2O3 and TiO2, promoted in materials microstructure in conjunction with the prosperity of phase, reached the object that improves corrosion-resistant property.Through test, though the applicable effect of these resistance to materials a little less than magnesia chrome brick, cost is significantly higher than magnesia chrome brick, cost factor has hindered the industrial applications of refractory materials.
The Chrome free refractories of magchrome refractory as an alternative, several refractory materialss such as magnalium matter, magnesium are calcareous for having of relating in research and development, magnesium titanium matter, magnesium zirconium matter, magnesium yttrium matter and magnesium carbonaceous, wherein of greatest concern is refractory magnesia-alumina material.These resistance to materials find that through using its wearing quality declines, and must improve raising to aspect performances such as the slag resistance of this system material and thermal shock resistances.Transient plastic phase processing is that the Barsoum M.W. that the U.S. must make every effort to overcome Xie Er (Drexel) university proposed in phase early 1990s, becomes TPPP (Transient Plastic Phase Process) technique.The plasticity of technique forebody performance metal impels pressed compact process to become plastic forming, but transient plastic phase processing do not stop to this, but metal further with compound or surrounding gas effect wherein, form new wild phase.Can roughly be expressed as: the transition plasticity phase matrix+reacting phase of " soft " → hard matrix+wild phase.The essence of technique is that the plasticity of performance metal makes it to become plastic forming, obtains fine and close green compact, and then metal converts wild phase to and matrix becomes high temperature resistant matrix.
Summary of the invention
The object of the invention is the above-mentioned deficiency for prior art, a kind of alumina-spinelle-corundum composite refractory material is provided.
Another object of the present invention is to provide the preparation method of this refractory materials.
Another object of the present invention is to provide the application of this refractory materials.
Object of the present invention can be achieved through the following technical solutions:
A kind of alumina-spinelle-corundum composite refractory material, comprise that (" % " represents mass percent by 1wt%～15wt%, take raw material total mass as benchmark, lower with) metallic aluminium powder, the magnesium-aluminium spinel of 5wt%～25wt% and the white fused alumina of 73wt%～90wt% or plate diamond spar in one or more compositions raw material and account for the inorganic bonding agent of the 1.5wt%～3wt% of described raw material total mass.
Wherein, one or more in inorganic bonding agent preferably phosphoric acid aluminum dihydrogen, Sodium hexametaphosphate 99 or tripoly phosphate sodium STPP.
The chemical constitution of alumina-spinelle-corundum composite refractory material of the present invention (mass percent) is: Al
2o
370%～90%, MgO15%～30%, Al 1%～15% and inevitably impurity.
Described alumina-spinelle-corundum composite refractory material, each raw material granularity grating is as follows:
The particle 45～50% (wt%) of 4-1mm coarsness;
The particle 15～25% (wt%) of granularity in 1-0mm;
The fine powder 30～35% (wt%) of≤0.088mm.
The preparation method of described alumina-spinelle-corundum composite refractory material:
(1) batching: weigh desired raw material according to proportioning claimed in claim 1;
(2) mix: by raw material fine powder premix 25min～35min of≤0.088mm, the raw material that granularity is greater than to 0.088mm is evenly poured in coating drum and is mixed, after 10min～20min, stop stirring, half of inorganic bonding agent poured into, continue to stir after 10min～20min, pre-mixed fine powder material is poured in coating drum and stirred 10min～20min, then remaining bonding agent is all poured into and continued to stir 35min～55min, stop stirring;
(3) ageing mixture: by the compound sealing mixing, fully ageing mixture is 8～24 hours;
(4) moulding: by compound 130Mpa～170Mpa compression moulding on pressing machine, maintenance 20～24h at 25～28 ℃, and at 100～110 ℃ dry 20～24h;
(5) thermal treatment: the refractory materials of moulding is incubated to 3～6 hours in 300 ℃～600 ℃ air atmospheres.
The ageing mixture time described in step (5) is relevant with temperature, and the ageing mixture time in spring, summer, autumn is preferably 8～10h, and the ageing mixture time in winter is preferably 20～24h.
The application of described alumina-spinelle-corundum composite refractory material in preparation RH refining furnace lining.
Corundum based refractory materials has good fire performance, anti-melting loss performance and slag penetration resistance energy, is applicable to various working conditionss, more common in vacuum treatment installation outside stove.Magnesium-aluminium spinel is as one of refractory materials important integral part, and it has good high-temperature behavior.From M-A binary phase diagram, can find out, magnesium-aluminium spinel is an intermediate product in this binary system, and it is by MgO: Al2O3=1: 1 forms, and fusing point is 2135 ℃.Corundum at high temperature can be solid-solubilized in magnesium-aluminium spinel, and solid solution capacity increases along with the rising of temperature, and when more than 1900 ℃, solid solution capacity can reach more than 20%.Compare with corundum, about better, the anti-FeO scouring of heat impedance is higher, Deformation velocity is at half.
The metallic aluminium of introducing mutually as transition plasticity, can make the apparent porosity of material significantly reduce, and plays the effect of plastic forming.Metallic aluminium fusing point is low, has good ductility, in soak process, as sintering agent, makes process become liquid phase sintering performance capillary force action, and by particle tension, material is inevitable finer and close, the raising that shows folding strength.Metallic aluminium easily at high temperature reacts generation aluminum oxide with oxygen, and this aluminium oxide active is good, in the resistance to material of alumina base, can be used as sintering aid.Under high temperature, metal A l atmosphere in nitrogen can generate the aluminium nitride with good erosion-resisting characteristics, when having carbon to exist, can generate dystectic carbide, to improving intensity and the resistance to fouling of goods, has active effect.
Effect advantage:
Main innovation of the present invention is take that corundum, spinel, metallic aluminium are raw material, does not introduce pollution of chromium and Prevent Carbon Contamination in secondary refining process; The fusing point low (being only 660 ℃) of the metallic aluminium adding, the transition plasticity phase matrix as " soft " in material is introduced, and by controlling its content, reaches the object of strongthener erosion-resisting characteristics; Needn't burn till by high temperature, reduce energy consumption, cost-saving, shorten the production cycle, quality and the life-span of having improved product.
The present invention is based on the raw materials of magnesium oxide resource of China's abundant, operating environment for RH refining furnace key position harshness, in corundum spinelle, introduce metallic aluminium powder, make full use of the advantage of transient plastic phase processing, research and develop the Chrome free refractories of excellent property, this refractory materials has with respect to RH lower channel high-quality MgO-Cr
2o
3fundamental Physical Properties and high-temperature behavior (table 1) that brick and existing other chromium-free bricks are more excellent, especially slag penetration resistance energy, its cost and high-grade magnesium chromium goods are suitable on RH equipment, thereby can substitute on a large scale the resistance to material of magnesium chromium that has contaminate environment, high energy consumption and resource scarcity problem, stablize controlled work-ing life, industry waste product reproducible utilization, reduces resistance to material waste and consumes.Better meet the requirement of ferrous metallurgy fast development and environment protection, this also will represent that following novel refractory is efficient, the developing direction of energy-saving and environmental protection simultaneously.
Table 1
Accompanying drawing explanation
Fig. 1 is MgO-Al
2o
3binary phase diagram.
Embodiment
Formula according to table 2 takes raw material, and each raw material granularity grating is as follows:
Particle 45～the 50wt% of 4-1mm coarsness;
Particle 15～the 25wt% of granularity in 1-0.088mm;
Be prepared as follows alumina-spinelle-corundum composite refractory material sample:
Alumina-spinelle-corundum composite refractory material
(1) batching: weigh desired raw material according to the proportioning in table 2;
(2) mix: by raw material fine powder premix 25～35min of≤0.088mm, the raw material (being aggregate) that granularity is greater than to 0.088mm is evenly poured in coating drum and is mixed, after 15min, stop stirring, half of inorganic bonding agent poured into, continue to stir after 15min, pre-mixed fine powder material is poured in coating drum and stirred 15min, then remaining bonding agent is all poured into and continued to stir 40min, stop stirring;
(3) ageing mixture: by the compound sealing mixing, abundant ageing mixture is 8～10 hours under the envrionment temperature of 25 ℃;
(4) moulding: compound 150Mpa (GB/T7321-2004) on pressing machine is pressed into the rectangular sample of 230mm * 114mm * 65mm, maintenance 24h at 25～28 ℃, and at 110 ℃ dry 24h;
(5) thermal treatment: the refractory materials of moulding is incubated to 5 hours in 300 ℃ of air atmospheres.
Sample after thermal treatment is carried out to the conventional physico-chemical properties such as apparent porosity (GB/T2997-2000), volume density (GB/T2997-2000), cold crushing strength (GB/T3997.2-1998), refractoriness under load (GB/T5989-1998) and detect, assay is in Table 3.
Table 2
Table 3
As can be seen from Table 3, in the increase along with aluminium content, the cold crushing strength of material increases to some extent, illustrates that aluminium has played the effect of Plastic Deformation phase, makes the improved performance of material.
Embodiment 2
Preparation method, with embodiment 1, produces alumina-spinelle-corundum composite refractory material according to the formula shown in table 4, and conventional physico-chemical properties detects in Table 5.
Table 4
Table 5
As can be seen from Table 5, during spinel content 15～20%, material apparent porosity is relatively low, but difference is little.
Claims (1)
1. alumina-spinelle-corundum composite refractory material, is characterized in that comprising by the metallic aluminium powder of 6wt%, the white fused alumina of the magnesium-aluminium spinel of 15wt% and 79 wt % or one or more raw materials that form in plate diamond spar and account for the inorganic bonding agent of the 1.5wt% ~ 3wt% of described raw material total mass; Described inorganic bonding agent is one or more in aluminium dihydrogen phosphate, Sodium hexametaphosphate 99 or tripoly phosphate sodium STPP; And prepare by the following method:
(1) batching: weigh desired raw material according to above-mentioned proportioning;
(2) mix: by raw material fine powder premix 25 min ~ 35min of≤0.088mm, the raw material that granularity is greater than to 0.088mm is evenly poured in coating drum and is mixed, after 10 min ~ 20min, stop stirring, half of inorganic bonding agent poured into, continue to stir after 10 min ~ 20min, pre-mixed fine powder material is poured in coating drum and stirred 10 min ~ 20min, then remaining bonding agent is all poured into and continued to stir 35 min ~ 55min, stop stirring;
(3) ageing mixture: by the compound sealing mixing, fully ageing mixture is 8 ~ 24 hours;
(4) moulding: by compound Mpa compression moulding in 130Mpa ~ 170 on pressing machine, maintenance 20 ~ 24h at 25 ℃ ~ 28 ℃, and at 100 ℃ ~ 110 ℃ dry 20 ~ 24h;
(5) thermal treatment: the refractory materials of moulding is incubated to 3 ~ 6 hours in 300 ℃ ~ 600 ℃ air atmospheres.
2, alumina-spinelle-corundum composite refractory material according to claim 1, is characterized in that raw material granularity grating is as follows:
The particle 45 wt % ~ 50 wt % of 4-1mm coarsness;
The particle 15 wt % ~ 25 wt % of granularity in 1-0.088mm;
The fine powder 30 wt % ~ 35 wt % of≤0.088mm.
3, the preparation method of alumina-spinelle-corundum composite refractory material claimed in claim 1, is characterized in that:
(1) batching: weigh desired raw material according to proportioning claimed in claim 1;
(2) mix: by raw material fine powder premix 25 min ~ 35min of≤0.088mm, the raw material that granularity is greater than to 0.088mm is evenly poured in coating drum and is mixed, after 10 min ~ 20min, stop stirring, half of inorganic bonding agent poured into, continue to stir after 10 min ~ 20min, pre-mixed fine powder material is poured in coating drum and stirred 10 min ~ 20min, then remaining bonding agent is all poured into and continued to stir 35 min ~ 55min, stop stirring;
(3) ageing mixture: by the compound sealing mixing, fully ageing mixture is 8 ~ 24 hours;
(4) moulding: by compound Mpa compression moulding in 130Mpa ~ 170 on pressing machine, maintenance 20 ~ 24h at 25 ℃ ~ 28 ℃, and at 100 ℃ ~ 110 ℃ dry 20 ~ 24h;
(5) thermal treatment: the refractory materials of moulding is incubated to 3 ~ 6 hours in 300 ℃ ~ 600 ℃ air atmospheres.
4, preparation method according to claim 3, is characterized in that the described ageing mixture time of step (5) is relevant with temperature, and the ageing mixture time in spring, summer, autumn is 8 ~ 10h, and the ageing mixture time in winter is 20 ~ 24h.
5, the application of alumina-spinelle-corundum composite refractory material claimed in claim 1 in preparation RH refining furnace lining.
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