CN103626503A - Longevous mullite brick for hot blast stove and preparation method thereof - Google Patents
Longevous mullite brick for hot blast stove and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a longevous mullite brick for a hot blast stove. The brick is prepared from the following raw materials in percentage by weight: 75-95% of mullite containing 70-80wt% of Al2O3, 0-20% of sillimanite and 4-6% of Guangxi white mud, and further comprises 2-4% of lignin based on total weight of the above three raw materials. The preparation method comprises the following steps: a, weighing the raw materials in proportion, and adding water, mixing and stirring to prepare a green brick; b, drying; and c, firing: the sintering temperature is 1380-1480 DEG C. The sillimanite is added into the mullite, so that the creep resistance of the brick can be remarkably improved. Particularly, the sillimanite is mullitized under a condition of a high temperature over 1400 DEG C and accompanies volume expansion, the expansion just can offset or partially offset contraction generated in the high-temperature using process, so that the material has good creep resistance.
Description
Technical field
The invention belongs to fire resisting material field, relate in particular to the mullite firebrick that a kind of hotblast stove is used.
Background technology
Iron And Steel Industry is occupied critical role in national economy, and blast furnace, hotblast stove are most important equipment in Iron industry.It is only about 8 years that blast furnace, the lifetime of hot-air stove of external advanced country can reach 15-20 Nian， China.Realize long service life, refractory materials is one of its key factor.
Along with the progress of smelting technology in recent years, hotblast stove has generally adopted high wind-warm syndrome technology, and requires the longer service life of hotblast stove, so the performance of refractory materials has been had to further requirement.High-Alumina brick is used in hotblast stove, and in hotblast stove, the environment of high temperature, high pressure is a very large test for the creep-resistant property of high alumina refractories, directly affects the work-ing life of hotblast stove.This is that while adopting common high alumina brick because of most of hotblast stoves high-temperature zone, erosion has in various degree appearred in its top checker brick, i.e. " scorification ", thus cause the hole of checker brick to stop up; Yet these high-temperature zone checker brick are also bearing the loading of top checker brick, main generation causes subsiding of checker brick because creep causes checker brick uneven subsidence; And the main phenomenon that position is damaged in hotblast stove top and pipeline junctions etc., be also by high-temperature creep resistance bad and cause brick phenomenon and vault ftractures.Adopt pure homogeneous fused mullite brick also to have above-mentioned defect, because pure homogeneous fused mullite brick is at 1300 ℃ and when following, there is good creep-resistant property, but when creep temperature is greater than 1300 ℃, show poor creep-resistant property.In the high-temperature zone of hotblast stove, its temperature is greater than 1300 ℃, therefore also there will be erosion in various degree.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, a kind of long-lived mullite brick and preparation method thereof for hotblast stove is provided, the present invention adds sillimanite in mullite, can significantly improve its creep-resistant property, particularly under more than 1400 ℃ hot conditionss, sillimanite generation mullitization, and be accompanied by volumetric expansion, and this expansion just can be offset or partial offset applied at elevated temperature process in the contraction that produces, make material there is good creep-resistant property.After creep, the volume density of sample all increases, and void content slightly declines.
For achieving the above object, the present invention is by the following technical solutions:
The long-lived mullite brick of hotblast stove, is prepared from by the raw material of following mass percent: containing Al
2o
3quality percentage amounts is mullite 75%-95% part of 70%-80%, sillimanite 0%-20% part, and Guangxi white clay 4%-6% part, also comprises the xylogen of the 2-4% of above three kinds of raw materials quality summations.
The long-lived mullite brick of above-mentioned hotblast stove, is prepared from by the raw material of following mass percent: containing Al
2o
3quality percentage amounts is 85% part of the mullite of 70%-80%, 10% part of sillimanite, and 5% part of Guangxi white clay, also comprises 3% xylogen of above three kinds of raw materials quality summations.
The long-lived mullite brick of above-mentioned hotblast stove, Al in described mullite
2o
3quality percentage composition is 75%.
The long-lived mullite brick of above-mentioned hotblast stove, mullite is high aluminium bauxite clinker homogenization material, wherein mullite macrobead 1-3mm, middle particle 0.075-1mm and fine powder fineness≤0.074mm are in mass ratio for 4:2:1.5-3.5 is obtained by mixing, sillimanite granularity is 0-0.2mm, and white clay particle is 0.070-0.088mm.
A preparation method for long-lived mullite brick for hotblast stove, comprises the following steps: a. takes each raw material by proportioning, adds water mix and blend, makes adobe; B. dry; C. fire: around junction temperature, be 1380 ℃-1480 ℃.
The preparation method of long-lived mullite brick for above-mentioned hotblast stove, the sintering temperature of described step c is 1430 ℃.
Adopt technique scheme, the present invention has following advantage: experimental result shows: pure homogeneous fused mullite brick, at 1300 ℃ and when following, has good creep-resistant property, but when creep temperature is greater than 1300 ℃, shows poor creep-resistant property.In mullite, add sillimanite, can significantly improve its creep-resistant property, particularly under more than 1400 ℃ hot conditionss, sillimanite generation mullitization, and be accompanied by volumetric expansion, and this expansion just can be offset or partial offset applied at elevated temperature process in the contraction that produces, make material there is good creep-resistant property.After creep, the volume density of sample all increases, and void content slightly declines.
Because mullite will be applicable to high-temperature use and have good sintering character, and it is little that it possesses particle diameter, on axle, the chemical uniformity that particle size distribution is narrow and purity, therefore there is good structure properties, chemical property, thermal characteristics and mechanical property, and sillimanite has at high temperature volumetric expansion, the non-shrinking permanent expansion performance of cooling rear volume, and can be under hot conditions the irreversible mullite that is converted into, in this reaction process, can cause certain volumetric expansion, can compensate the draught that high temperature load brings, and then the creep-resistant property of raising high alumina brick, the phase transformation of sillimanite simultaneously transforms the weave construction of also having improved high alumina brick, its crystallization direction of mullite after phase transformation is parallel to former crystalline phase interface, can effectively suppress Grain Boundary Sliding, further improve the creep-resistant property of brick.
Hotblast stove mainly adopts the sillimanite that adds different content in mullite to improve the creep-resistant property of high alumina products with novel mullite brick of long lifetime, and then prepares the mullite brick sample of different sillimanite content.
Accompanying drawing explanation
Fig. 1 is the crystalline structure of mullite.
Fig. 2 is the crystalline structure of sillimanite.
Fig. 3 is the sillimanite crystalline structure with the performance of coordination polyhedron form.
Fig. 4 is sillimanite thermal expansion curve.
Fig. 5 is the relation of sillimanite content and void content, volume density.
Fig. 6 is sillimanite content and compressive strength relation.
Fig. 7 is sillimanite content and refractoriness under load.
Fig. 8 is embodiment 4 microstructures.
Fig. 9 is sample embodiment 5 micro-structure diagrams.
Figure 10 is sample embodiment 6 microstructures.
Figure 11 is the undecomposed sillimanite energy spectrum analysis of embodiment 6 figure.
Figure 12 is the ongoing sillimanite energy spectrum analysis of embodiment 6 mullitization figure.
Figure 13 is that embodiment 6 sillimanites decompose the energy spectrum analysis figure while producing mullite.
Figure 14 is the XRD material phase analysis of different sillimanite content samples.
Embodiment
A preparation method for long-lived mullite brick for hotblast stove, comprises the following steps: a. takes the preparation raw material of following mass percent: containing Al
2o
3quality percentage amounts is mullite 75%-95% part of 70%-80%, sillimanite 0%-20% part, Guangxi white clay 4%-6% part; Take again the xylogen of the 2-4% of above three kinds of raw materials quality summations; Add water mix and blend, make adobe; B. dry; C. fire: around junction temperature, be 1380 ℃-1480 ℃, optimum sintering temperature is 1430 ℃.
Mullite of the present invention is high aluminium bauxite clinker homogenization material, wherein mullite macrobead 1-3mm, middle particle 0.075-1mm and fine powder fineness≤0.074mm are in mass ratio for 4:2:1.5-3.5 is obtained by mixing, sillimanite granularity is 0-0.2mm, and white clay particle is 0.070-0.088mm.
The present invention is to adopt Al in mullite
2o
3quality percentage composition is 75% to describe for example.
Table 1 is the embodiment list of embodiments of the invention 1-3
Table 1
Table 2 is embodiment lists of embodiments of the invention 4-6
Table 2
Table 2 is embodiment lists of embodiments of the invention 4-6
the Performance Detection of embodiment 4-6
The traditional performance of sample detects and comprises: the apparent porosity of sample, volume density, cold crushing strength, refractoriness under load, high temperature creep rate, X-ray diffraction material phase analysis and surface sweeping electron microscopic contextual analysis of organization.
1. volume density and apparent porosity: sample is adopted to the detection method of GB/T2997-1982 regulation, weigh the quality of sample, then measure its volume with hydrostatic weighing method, calculate apparent porosity, volume amasss density
2. cold crushing strength: sample is adopted to the detection method of GB/T5072-1985 regulation, under room temperature, the speed with pressure testing machine with regulation, the sample loading to specified dimension, until sample is broken.According to the area of recorded ultimate load and sample carry load, calculate cold crushing strength.
3. refractoriness under load: the detection method that sample is adopted to YB/T370-1995 regulation.The refractoriness under load of refractory materials depends primarily on minerals commonly used in chemical industry composition, granulometric composition, the crystalline texture of raw material, and the ratio of crystalline phase and glassy phase, glassy phase viscosity with temperature raise and situation about changing and the heat-up rate while measuring etc.The softening temperature of crystalline phase, should approach its temperature of fusion, because viscous deformation likely occurs while only having the temperature of fusion of approaching crystalline phase.But refractory materials still has eutectic except crystalline phase, and these eutectics are fused into liquid phase at a certain temperature, this temperature, far below the softening temperature of crystalline phase, has so just reduced the refractoriness under load of ceramic refractory.
The mensuration of refractory product refractoriness under load is generally under the seating load of 0.2MPa, with certain heat-up rate homogeneous heating, and temperature when mensuration sample compresses 0.6%, 4%, 40%.The loading softening that texturing temperature when sample compresses 0.6% is sample starts temperature, i.e. usually said load softening point.
High temperature load softening temperature can show structural strength and the deformation of refractory product under the condition close with its service condition to a certain extent, because of but the important performance indexes of refractory product.
4. high temperature creep rate: the detection method that sample is adopted to GB/T 5073-1985 regulation.
5. utilize X-ray diffractometer to carry out material phase analysis to sintered specimen; Utilize scanning electronic microscope to carry out contextual analysis of organization to sintered specimen.
The research of the traditional performance of 3 samples
3.1 apparent porosities and volume density
1. experimental result
The apparent porosity of test brick and volume density are as shown in table 3.1.
Table 3.1 test brick void content & volume density
2. interpretation of result
Fig. 5 is the graph of a relation of volume density, apparent porosity and the sillimanite content of sample, and as can be seen from the figure, along with the increase of sillimanite content, the volume density of sample reduces gradually, and apparent porosity increases gradually.Reducing of the volume density of sample is that process due to sillimanite mullitization can produce volumetric expansion, and again because the density of mullite is less than sillimanite, therefore the volume density of whole sample reduces simultaneously, and void content raises.
3.2 cold crushing strength
1. experimental result
The compressive strength of test brick is as shown in table 3.2.
Table 6 is embodiment 4-6 brick compressive strengths
2. interpretation of result
Fig. 6 is the cold crushing strength of sample and the graph of a relation of sillimanite content, as can be seen from the figure, increase along with sillimanite content, cold crushing strength reduces gradually, this is because of the increase along with sillimanite content, refractory materials has larger void content and lower volume density, so its compressive strength also reduces along with the increase of sillimanite content.
refractoriness under load
1. experimental result
The refractoriness under load of test brick is as shown in table 3.3.
Table 3.3 test brick refractoriness under load
2. interpretation of result
Fig. 7 is the refractoriness under load of sample and the graph of a relation of sillimanite content, as can be seen from the figure, increase along with sillimanite content, refractoriness under load raises gradually, this is owing to can carrying out mullitization under sillimanite high temperature, and the structure of the needle-like forming after its mullitization, long column shape causes it to have higher refractoriness under load.And again because the density of sillimanite is greater than mullite, therefore, sillimanite itself just has the high-temperature behavior that is better than mullite, adds the amount of sillimanite more, its high-temperature behavior is better.
Fig. 8 has provided embodiment 4(and has not added sillimanite) scanning electron microscope diagram.From micro-structure diagram, can find out, embodiment 4 structures are comparatively fine and close, have lower void content.From energy spectrogram and analytical results, be almost wherein mullite structure entirely, therefore also confirmed macroscopical upper its higher compressive strength.
The add-on that Fig. 9 has provided embodiment 5(sillimanite is 10%) scanning electron microscope diagram.From can spectrogram and analytical results, in sample, there is a little corundum to exist mutually, analyzing its reason may be due to, and raw material is not realized complete homogenizing, also contains part corundum, so corundum is incorporated in sample by raw material except mullite.
The add-on that Figure 10 has provided sample embodiment 6(sillimanite is 20%) scanning electron microscope diagram.
Figure 11, Figure 12 and Figure 13 are the energy spectrum analysis in embodiment 6, and Figure 11 is undecomposed sillimanite energy spectrum analysis figure, and Figure 12 place is the ongoing sillimanite energy spectrum analysis of mullitization figure, and Figure 13 place is that sillimanite decomposes the energy spectrum analysis figure while producing mullite.
the material phase analysis of embodiment 4-6
Figure 14 is the XRD material phase analysis of embodiment 4, embodiment 5, embodiment 6, and as can be seen from the figure, in embodiment 4, main phase is mullite phase and corundum phase.Wherein principal crystalline phase is mullite, is secondly corundum phase.In embodiment 5 samples, main phase is mullite phase, corundum phase and sillimanite phase.From figure, can draw, the principal crystalline phase in embodiment 5 samples is mullite phase, but mullite phase proportion does not have the ratio in embodiment 4 large, is secondly undecomposed sillimanite phase and a small amount of corundum phase.In embodiment 6 samples, main phase is also mullite phase, corundum phase and sillimanite phase, and just mullite phase proportion is lower than two other sample, but sillimanite phase proportion will be higher than embodiment 5 samples.
Raw of the present invention is selected
One, mullite is main raw material, employing be Al
2o
3content is 75% mullite, and granularity has coarse particles 3-1mm, middle particle 1-0mm and fine powder fineness≤0.074mm.
Two, auxiliary material mainly contains sillimanite 0-0.2mm, Guangxi white clay 0.074mm.
Additional bonding agent is xylogen.
The structure and properties of mullite:
Al in pure mullite
2o
3content between 62%～100%, the Al of pure mullite
2o
3content is about 71.8%, for high aluminium material, belong to rhombic system, average structure is connected to the chain of parallel c-axis by [AlO6] octahedra rib altogether, be positioned at the 4 Ge Jiaodinghe centers on unit cell (001) projection plane, at the Z=1/2 place (Z=1/2 that is equivalent to sillimanite unit cell, 3/4 place) of each unit cell, octahedra chain is connected with [AlO4] tetrahedron with [SiO4], and tetrahedron forms two strands and is also parallel to c-axis.Tetrahedron bridging oxygen position and other Sauerstoffatom will lose, and in tetrahedron, remaining Sauerstoffatom and T position Al and Si ion are subjected to displacement, and are meanwhile accompanied by Al in limbs and replace Si(Fig. 1).The unit cell parameters Co value of mullite is half of sillimanite Co value, can release thus the ordered distribution of Al and Si in sillimanite tetrahedron, and the Al in mullite tetrahedron and Si are unordered.
Mullite structure is catenation, so its crystal is long column shape, the needle-like of extending along c-axis, in high alumina products, these acicular mullites are the firm skeleton of interspersed formation mutually, in its structure, [AlO6] octahedron has played stable skeleton supporting role, thereby mullite is very stable, and there are a series of good performances.As: its fusing point is 1870 ℃, and proportion is 3.03, and hardness is 6.7, and polar expansion is little.In the time of 20～1000 ℃, be 5.3x10-6/degree, thermal conductivity is 13.8 kilojoules/ meter Shi Du.Young's modulus is low, is 160～200Gpa, is about Al2O3, half of SiC, chemical resistance of concrete, high temperature creep-resisting, good thermal shock.
2.1.2 the structure and properties of sillimanite
The crystalline structure of sillimanite as shown in Figures 2 and 3.Sillimanite has at high temperature volumetric expansion, the non-shrinking permanent expansion performance of cooling rear volume, and at high temperature (1500～1550 ℃) are irreversibly converted into mullite and cristobalite, are attended by certain volumetric expansion simultaneously.With the rising of temperature, the polar expansion of sillimanite changes visible Fig. 4.
As shown in Figure 4, because pure sillimanite mineral are before Mullite-Crystallization conversion starts, because of without decomposition reaction or transformation of crystal, be that general physicals shows, therefore its expansion curve is without obvious variation.After temperature rises to Mullite-Crystallization is started, along with the variation of temperature, just there is rising sharply in expansion curve, and rate of expansion enlarges markedly (seeing A in Fig. 4).When sillimanite mineral contain a certain amount of impurity, its rate of expansion there will be the variation (seeing B in Fig. 4) of ups and downs.Find out thus, when in sample ore, the high and quality of sillimanite mineral content is good again, it just has good high-temperature behavior.
Sillimanite is the high alumina refractory of typical pyrometamorphism mineral and high-quality, and composition is Al
2o
3siO
2, Al wherein
2o
362.9%, SiO
237.1%.When high-temperature calcination, in 1545 ℃, be converted into mullite and separate out SiO
2, formed mullite is identical with the orientation of original sillimanite.Its refractoriness is greater than 1830 ℃, and hardness is greater than 7, proportion 3.25.There is good thermostability, wear resistance, good thermal property and the higher intensity such as chemical resistance of concrete, high temperature creep temperature height, sillimanite goods are taken out to put into continuously water several times cooling 1200 ℃ time, and can not crack or occur bursting phenomenon, and its physicochemical property is better than common high alumina products, even can match in excellence or beauty with corundum products.And in fact general sillimanite goods, and even complex-shaped goods, in the preparation technology of refractory materials, be also comparatively simple.It does not have SiO
2the large expansion of formula, does not have the aquation of MgO; The large fragility that there is no chromium goods.Even if use clay as bonding agent, its contraction of burning till is also very little.So be widely used in the industrial circles such as metallurgical furnace, high temperature material of construction, technical ceramics, silumin, steel fiber, it is the important source material of producing high alumina products.
The character of table 2.2 andaluzite, kyanite and sillimanite mineral
The pyrolytic conversion performance of table 2.3 three stones
Claims (7)
1. the long-lived mullite brick of hotblast stove, is prepared from by the raw material of following mass percent: containing Al
2o
3quality percentage amounts is the mullite 75%-95% of 70%-80%, sillimanite 0%-20%, Guangxi white clay 4%-6%; The xylogen that also comprises the 2%-4% of above three kinds of raw materials quality summations.
2. the long-lived mullite brick of hotblast stove according to claim 1, is characterized in that: the raw material by following mass percent is prepared from: containing Al
2o
3quality percentage amounts is the mullite 85% of 70%-80%, sillimanite 10%, and Guangxi white clay 5%, also comprises 3% xylogen of above three kinds of raw materials quality summations.
3. the long-lived mullite brick of hotblast stove according to claim 1 and 2, is characterized in that: Al in described mullite
2o
3quality percentage composition be 75%.
4. the long-lived mullite brick of hotblast stove according to claim 3, it is characterized in that: mullite is high aluminium bauxite clinker homogenization material, wherein mullite macrobead 1-3mm, middle particle 0-1mm and fine powder fineness≤0.074mm are in mass ratio for 4:2:1.5-3.5 is obtained by mixing, sillimanite granularity is 0-0.2mm, and white clay fineness is 0.070-0.080mm.
5. according to the long-lived mullite brick of hotblast stove according to claim 3, it is characterized in that: sillimanite granularity is 0-0.2mm, white clay fineness is 0.074mm.
6. a preparation method for long-lived mullite brick for hotblast stove claimed in claim 1, is characterized in that: comprise the following steps: a. takes each raw material by proportioning, adds water mix and blend, makes adobe; B. dry; C. fire: around junction temperature, be 1380 ℃-1480 ℃.
7. the preparation method of long-lived mullite brick for hotblast stove according to claim 3, is characterized in that: the sintering temperature of described step c is 1430 ℃.
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| CN108675804A (en) * | 2018-06-08 | 2018-10-19 | 郑州凯翔耐火材料有限公司 | A kind of highly heatproof and shockproof mullite brick and its production technology |
| CN108794031A (en) * | 2018-08-29 | 2018-11-13 | 通达耐火技术股份有限公司 | A kind of cement kiln low-aluminum mullite brick and preparation method thereof |
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| CN112457031A (en) * | 2020-12-10 | 2021-03-09 | 郑州凯翔耐火材料有限公司 | Low-creep high-alumina brick and preparation method thereof |
| CN113480301A (en) * | 2021-07-15 | 2021-10-08 | 山东淄博沈淄耐火材料有限公司 | Preparation method of large brick at bottom of high-temperature sillimanite pool of large float glass melting furnace |
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| CN115490505A (en) * | 2022-11-02 | 2022-12-20 | 中钢洛耐科技股份有限公司 | Anti-scouring mullite runner brick and preparation method thereof |
| CN116516117A (en) * | 2023-04-12 | 2023-08-01 | 无锡环宇精密铸造有限公司 | Heat treatment process of super duplex stainless steel casting |
| CN116516117B (en) * | 2023-04-12 | 2023-09-19 | 无锡环宇精密铸造有限公司 | Heat treatment process of super duplex stainless steel casting |
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