CN112456974A - Magnalium spinel brick for co-processing cement kiln and preparation method and application thereof - Google Patents

Magnalium spinel brick for co-processing cement kiln and preparation method and application thereof Download PDF

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CN112456974A
CN112456974A CN202011452149.5A CN202011452149A CN112456974A CN 112456974 A CN112456974 A CN 112456974A CN 202011452149 A CN202011452149 A CN 202011452149A CN 112456974 A CN112456974 A CN 112456974A
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magnesia
alumina spinel
flotation
magnesite
alumina
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CN112456974B (en
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康剑
马淑龙
马飞
王治峰
高长贺
张积礼
倪高金
周新功
孔祥魁
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Beijing Jinyu Tongda Refractory Technology Co ltd
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Beijing Jinyu Tongda Refractory Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—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
    • C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • C04B35/043—Refractories from grain sized mixtures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Abstract

The invention belongs to the technical field of refractory materials, and particularly relates to a magnesium aluminate spinel brick for a co-processing cement kiln, and a preparation method and application thereof. The magnesia-alumina spinel brick is prepared by using flotation magnesia, high-purity magnesia and electric melting magnesia-alumina spinel as main raw materials and performing high-temperature treatment; the mass ratio of the flotation magnesia to the high-purity magnesia to the fused magnesia-alumina spinel is (54-65): (18-28): (12-25). The magnesia-alumina spinel brick not only has proper normal-temperature compressive strength and refractoriness under load, but also has higher volume density and lower apparent porosity, has higher sintering densification degree, can effectively reduce the permeation of aggressive substances, and has better erosion resistance; meanwhile, the thermal shock resistant alloy has higher thermal shock stability, high-temperature rupture strength and high-temperature toughness; the magnesia-alumina spinel brick has excellent performance, low cost and high cost performance, so that the magnesia-alumina spinel brick has wider application range.

Description

Magnalium spinel brick for co-processing cement kiln and preparation method and application thereof
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a magnesia-alumina spinel brick and a preparation method and application thereof.
Background
The kiln lining is made of refractory material embedded in the inner surface of the rotary kiln cylinder body, and has the functions of protecting the cylinder body from being damaged by high temperature, insulating heat and reducing heat dissipation loss. The long-term safe operation of the rotary kiln is one of the main measures for increasing production and saving in the cement industry, and the long service life of the kiln liner directly influences the long-term safe operation of the rotary kiln.
The magnesia-alumina spinel brick used in the current market has larger porosity, lower volume density and poorer high-temperature toughness, and shortens the service life of the magnesia-alumina spinel brick on a co-processing cement kiln. Along with the development of the co-processing cement technology, the application of a large amount of industrial wastes and the like to replace raw fuels increases the circulation amount of alkali, chlorine and sulfur in the cement kiln, so that the erosion degree of the refractory material of the kiln lining is further intensified; meanwhile, the movement of bricks and the deformation of the kiln shell caused by the mechanical stress of the cement kiln also pose a serious challenge to the high-temperature toughness of the kiln lining refractory material.
CN103274711A discloses a high-strength low-conductivity magnesia-alumina spinel brick, which takes a magnesia-alumina synthetic material with specific granularity and fused magnesia as raw materials, and the magnesia-alumina spinel brick obtained by sintering is suitable for a cement rotary kiln, and has excellent sintering performance, thermal shock stability, erosion resistance and permeability resistance. However, in practical use, the alloy has poor toughness (the number of water-cooling thermal shocks is more than 13), large porosity (26%), low volume density (2.6 g/cm)3) And the like, so that the method cannot well cope with the current situations that the corrosion of the kiln lining refractory material is increased and the mechanical stress of the cement kiln damages the kiln lining refractory material due to the replacement of raw materials in the co-processing cement kiln.
CN110790579A discloses a chromium-free refractory brick, which is prepared by adding various raw materials such as high-purity magnesite, hercynite and cosolvent to adjust the solution viscosity in cement clinker on the surface of a refractory material and reduce the temperature generated by a liquid phase, so that the refractory material has good kiln coating hanging property and thermal shock resistance and good flexibility. However, the refractory material has the defects of more raw material types, complex production process, higher cost and the like, and in addition, iron in the refractory material can be adversely affected due to price change, for example, researches of Lihongxia and the like find that the refractory material contains Fe2O3The spinel brick is only suitable for kilns with stable atmosphere and low load in the kiln.
CN107117976A discloses a magnesia-alumina spinel brick for a cement kiln transition zone and a preparation method thereof, belonging to the field of refractory materials, the raw materials comprise sintered magnesia and fused magnesia-alumina spinel, calcium lignosulfonate solution is used as a bonding agent, various raw materials are weighed according to the proportion during production, mixed uniformly to obtain a mixture, pressed and formed, dried for 25-35h at 100-200 ℃, and sintered in a 1550-. The product of the invention has high volume density and strength, good thermal shock stability, erosion resistance, abrasion resistance and high refractoriness under load. However, the impurity content of the sintered magnesite raw material is high, the improvement of the high-temperature toughness of the product is not facilitated, the cost of the raw material is high, and the calcium lignosulfonate, which is a bonding agent used in the production, can emit sulfur oxides in the production process, and causes environmental pollution if the sulfur oxides are not properly treated. In addition, the product index apparent porosity of the product obtained by the preferred embodiment is 16.6 percent which is higher than the apparent porosity of the product obtained by the preferred embodiment in this respect of 14.5 percent, and the volume density is 2.94g/cm3A bulk density of 3.03g/cm lower than that of the preferred embodiment3And the service life of the co-processing cement kiln can be shortened due to the lower high-temperature breaking strength of 3.45 MPa.
Disclosure of Invention
The invention aims to provide a magnesia-alumina spinel brick for a co-processing cement kiln, which not only has proper normal-temperature compressive strength and refractoriness under load, but also has higher volume density and lower apparent porosity, higher sintering densification degree, effective reduction of permeation of aggressive substances and better erosion resistance; meanwhile, the thermal shock resistant alloy has higher thermal shock stability, high-temperature rupture strength and high-temperature toughness; the magnesia-alumina spinel brick has excellent performance, low cost and high cost performance, so that the magnesia-alumina spinel brick has wider application range.
The magnesia-alumina spinel brick is prepared by using flotation magnesia, high-purity magnesia and electric melting magnesia-alumina spinel as main raw materials and performing high-temperature treatment;
the mass ratio of the flotation magnesia to the high-purity magnesia to the fused magnesia-alumina spinel is (54-65): (18-28): (12-25).
The flotation magnesite is prepared by flotation of low-grade magnesite, and has the advantages of high volume density, high purity, low price and the like; however, in the research, the burnt magnesite crystals after flotation have the characteristics of larger crystal size, more intercrystalline macropores, irregular shape of pores and the like compared with the same-grade sintered magnesite; meanwhile, the content of silicon in the magnesite after flotation is reduced, so that intergranular calcium oxide possibly exists as free calcium, and the high-temperature performance of the product, such as thermal shock resistance and high-temperature fracture resistance, is poor when the magnesite is compounded as a raw material. And a certain amount of large pores existing between the crystal grains can also reduce the corrosion resistance of the product when the product is used as a raw material for compounding, such as the corrosion resistance of cement kiln alkali, chlorine, sulfur, sulfate and the like, and further influence the service performance of the product.
Therefore, after intensive research, high-purity magnesite, fused magnesia-alumina spinel and calcined alumina are selected and compounded, the mass ratio of the high-purity magnesite, the fused magnesia-alumina spinel and the calcined alumina is controlled, and the thermal mismatch mechanism of in-situ magnesia-alumina spinel formed by flotation magnesite and calcined alumina is fully utilized, so that the problems existing in flotation magnesite as a raw material are solved, and the advantages of high volume density, high purity and the like of the flotation magnesite are fully exerted. The magnesium aluminate spinel brick has low porosity and high volume density, and also has good high-temperature toughness, erosion resistance and thermal shock stability, so that the contradiction that the quite high porosity is required to be reserved for improving the thermal shock stability in the research and development of kiln lining refractory materials is improved, and the strength and the erosion resistance of the materials are reduced.
Preferably, the mass ratio of the flotation magnesia to the high-purity magnesia to the electric smelting magnesia-alumina spinel is (54-60): (19-28): (13-22).
Preferably, the indices of each main raw material are as follows:
the main indexes of the flotation magnesite are as follows: the MgO content is 97.63%, SiO2The content is less than or equal to 0.5 percent, the CaO content is less than or equal to 1.0 percent, and the volume density is more than or equal to 3.3g/cm3The granularity is 200 meshes.
The main indexes of the high-purity magnesite are as follows: al (Al)2O3The content is less than or equal to 0.1 percent, the content of MgO is more than or equal to 97 percent, and SiO2The content is less than or equal to 1.0 percent, the CaO content is less than or equal to 1.5 percent, and the granularity is 180 meshes.
The main indexes of the electric melting magnesia-alumina spinel are as follows: al (Al)2O3The content is more than or equal to 65 percent, the content of CaO is less than or equal to 1.0 percent, the content of MgO is more than or equal to 30 percent, and the content of SiO is2The content is less than or equal to 0.5 percent, and the volume density is more than or equal to 3.3g/cm3。
Further research shows that the magnesia-alumina spinel brick with higher densification degree can be prepared by controlling the grain size distribution of the main raw materials, the porosity of the product is reduced, and the high-temperature toughness and high-temperature service performance of the product are improved, so that the problems of corrosion of alkali, chlorine, sulfur and sulfate in a cement kiln and damage of the cement kiln to the refractory of a kiln lining due to mechanical stress in the use process of the refractory are solved.
Preferably, the granularity grading of the flotation magnesite is controlled as follows: 7% of flotation magnesite with the thickness of 5-3 mm, 22% of flotation magnesite with the thickness of 3-1 mm and 25% of flotation magnesite with the thickness of 1-0 mm.
Preferably, the grain size distribution of the fused magnesia-alumina spinel is controlled as follows: 13% of 3-1 mm electric melting magnesia-alumina spinel and 5% of 1-0 mm electric melting magnesia-alumina spinel.
As one of the preferred embodiments of the invention, the particle size distribution and the mass percentage of part of raw materials are as follows: 7-8% of flotation magnesite with the granularity of 5-3 mm, 20-28% of flotation magnesite with the granularity of 3-1 mm and 23-28% of flotation magnesite with the granularity of 1-0 mm; 7-13% of fused magnesia-alumina spinel with the granularity of 3-1 mm and 2-7% of fused magnesia-alumina spinel with the granularity of 1-0 mm.
In order to further improve the performance of the refractory material, the raw material also comprises calcined alumina powder. Along with the increase of the addition amount of the calcined alumina powder, the apparent porosity of the obtained magnesia-alumina spinel brick is further reduced, the volume density is further improved, but the addition amount of the calcined alumina powder is not more than 10% of the total mass of the raw materials, otherwise, the kiln coating hanging performance of the magnesia-alumina spinel brick is easily reduced in the use process due to the increase of the melt viscosity, and the service life of the material is shortened.
The main indexes of the calcined alumina powder are as follows: al (Al)2O3The content is more than or equal to 99 percent, and the granularity is 325 meshes.
Preferably, the mass ratio of the flotation magnesite, the high-purity magnesite, the electric melting magnesia-alumina spinel to the calcined alumina powder is (54-56): (19-26): (18-20): (2-9).
As one of the preferred embodiments of the invention, the particle size distribution and the mass percentage of part of raw materials are as follows: 7-8% of flotation magnesite with the granularity of 5-3 mm, 22-24% of flotation magnesite with the granularity of 3-1 mm and 25-28% of flotation magnesite with the granularity of 1-0 mm; 10-13% of fused magnesia-alumina spinel with the granularity of 3-1 mm and 5-7% of fused magnesia-alumina spinel with the granularity of 1-0 mm.
The feedstock also includes a binder. The binding agent is water-soluble dextrin solution with specific gravity of 1.22-1.23g/cm3。
The second purpose of the invention is to provide a preparation method of the magnesia-alumina spinel brick.
The preparation method of the magnesia-alumina spinel brick comprises the following steps: mixing the raw materials, pressing, drying and sintering;
wherein the mixing process comprises: mixing the floated magnesite and the fused magnesia-alumina spinel particles, and then mixing the mixture with a binding agent to form a mixture A; and mixing the high-purity magnesite with the mixture A to obtain a mixed material.
The research finds that simply and directly mixing the main raw materials at one time can cause the problems of uneven materials, poor particle wrapping and the like, and is not beneficial to the later forming process and the improvement of the product performance; through repeated tests, the mixing sequence is finally determined to be adopted, the obtained materials are more uniform, the particle wrapping degree is better, and further the later-stage forming rate and the product performance are improved.
Preferably, the calcined alumina powder is mixed with the high purity magnesite before being mixed with the mixture a.
Preferably, the sintering temperature is controlled to be 1600-1700 ℃, the high temperature is kept constant for 3-4 hours, and the total sintering time is 140-180 hours. By controlling the conditions, the materials are combusted more fully, and the comprehensive performance of the obtained product is better.
Preferably, the pressing is performed with a 630 ton or 1000 ton press.
Preferably, the drying temperature is controlled to be 110-130 ℃, so that the subsequent processes can be smoothly carried out.
The third purpose of the invention is to provide a magnesia-alumina spinel brick, which comprises the following components in percentage by weight: 81-85% of MgO and Al2O312-17％，CaO≤0.95％，SiO2≤0.49％。
The fourth purpose of the invention is to provide the application of the magnesia-alumina spinel brick in refractory materials.
Preferably, the magnesia-alumina spinel brick is applied to a kiln liner of a co-disposal cement kiln.
The application of the magnesia-alumina spinel brick in a transition zone and a burning zone of a rotary cement kiln is further preferred.
The magnesia-alumina spinel brick has excellent high-temperature toughness, erosion resistance and thermal shock stability, the service life of the magnesia-alumina spinel brick reaches more than 24 months, the operation rate of a cement rotary kiln can be effectively improved, and the service life of a cylinder body is prolonged.
Compared with the prior art, the invention has the beneficial effects that:
the flotation magnesite grain is compounded with high-purity magnesite and fused magnesia-alumina spinel, so that the defect of poor high-temperature toughness caused by the existence of free calcium in the flotation magnesite is overcome, and the influence of inter-crystal irregular air holes on the erosion resistance is avoided. Therefore, the advantage of high volume density of the flotation magnesia is fully utilized, so that the sintering densification degree of the magnesia-alumina spinel brick is higher, and the penetration of aggressive substances can be effectively reduced; meanwhile, the lower SiO content in the magnesia-alumina spinel brick2And the content of CaO impurities reduces the formation of low-temperature phases in the material, and improves the thermal shock stability of the material.
Furthermore, calcined Al is introduced2O3The fine powder may be in a matrixThe spinel with uniform distribution is formed in situ, and can form large crystals or self-crystals with the pre-synthesized spinel in the matrix along with the increase of the content of the spinel, and the spinel is directly combined with periclase, so that the porosity of the refractory material is further reduced, the volume density of the refractory material is improved, and the thermal shock stability and the high-temperature toughness of the material are further improved.
In conclusion, the magnesia-alumina spinel brick is more suitable for being used in a co-disposal cement kiln, and the service life of the magnesia-alumina spinel brick is greatly prolonged; meanwhile, the method has good application prospect due to simple and environment-friendly production process, low price and higher cost performance.
Drawings
FIG. 1 shows different calcined Al2O3The introduction amount of the fine powder gives a high temperature bending resistance curve of the refractory.
FIG. 2 shows the thermal shock morphology of the refractory materials obtained in the different examples.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the following examples:
the double helix pre-mixer is a VSH-2C/B type double helix cone stirrer, and is purchased from Shanghai Shenyin machinery (group) Co.
The intensive mixer is an R19 inclined intensive mixer, and is purchased from Jian Hu Shenjiang machinery Co.
The press was an electric screw press of type HLDS-630T/B, available from Zhengzhou Hualong machines, Inc.
The raw material indexes adopted in the following examples are as follows:
flotation of magnesite: the MgO content is 97.63%, SiO2The content is less than or equal to 0.5 percent, the CaO content is less than or equal to 1.0 percent, and the volume density is more than or equal to 3.3g/cm3。
Electric melting magnesia-alumina spinel: al (Al)2O3The content is more than or equal to 65 percent, the content of CaO is less than or equal to 1.0 percent, the content of MgO is more than or equal to 30 percent, and the content of SiO is2The content is less than or equal to 0.5 percent, and the volume density is more than or equal to 3.3g/cm3。
The high-purity magnesite is prepared by the following steps: particle size of 180 mesh, Al2O3The content is less than or equal to 0.1 percent, the content of MgO is more than or equal to 97 percent, and SiO2The content is less than or equal to 1.0 percent, and the content of CaO is less than or equal to 1.5 percent.
The calcined alumina powder: al (Al)2O3The content is more than or equal to 99 percent, and the granularity is 325 meshes.
The above raw materials were purchased from Kaifeng and Kaifeng inorganic non-Material Co.
Example 1 (non-calcined alumina powder)
The embodiment provides a flotation magnesite thermal mismatch toughened low-impurity magnesia-alumina spinel brick, which is prepared from the following components in percentage by weight and a water-soluble dextrin solution (specific gravity 1.2) accounting for 2.2% of the total weight of the following components:
54% of flotation magnesite with the MgO content of 97.63%, 18% of fused magnesia-alumina spinel and 28% of high-purity magnesite powder, wherein 7% of flotation magnesite with the thickness of 5-3 mm, 22% of flotation magnesite with the thickness of 3-1 mm and 25% of flotation magnesite with the thickness of 1-0 mm; 13% of 3-1 mm electric melting magnesia-alumina spinel and 5% of 1-0 mm electric melting magnesia-alumina spinel.
The preparation method of the flotation magnesite thermally mismatched toughened low-impurity magnesia-alumina spinel brick comprises the following steps:
a. weighing the raw materials according to the proportion, placing 5.4kg of the flotation magnesia particles and 1.8kg of the raw materials of the electric melting magnesia-alumina spinel particles in a powerful mixing roll to mix for 2 minutes, and then adding 220ml of water-soluble dextrin solution to mix for 4 minutes;
b. adding 2.8kg of high-purity magnesite fine powder serving as a fine powder raw material into the mixture a, and premixing for 15 minutes to obtain a mixed material;
c. b, adding the mixed material obtained in the step b into an assembled die, and pressing and forming by adopting a 630-ton press to obtain a green brick;
d. drying in a drying kiln for more than 24 hours, wherein the inlet temperature of the drying kiln is less than 70 ℃, and the highest drying temperature is controlled to be 110-130 ℃.
e. And (3) sintering in a box-type resistance furnace at 1600 ℃ for 4 hours at high temperature, wherein the total sintering time is 140-180 hours.
Example 2 (without calcined alumina powder) (M2)
A flotation magnesite thermal mismatch toughened low-impurity magnesia-alumina spinel brick is prepared from the following components in percentage by weight and a water-soluble dextrin solution (the specific gravity is 1.2) accounting for 2.2 percent of the total weight of the following components:
54% of flotation magnesite with the MgO content of 97.63%, 18% of fused magnesia-alumina spinel and 28% of high-purity magnesite powder, wherein 7% of flotation magnesite with the thickness of 5-3 mm, 22% of flotation magnesite with the thickness of 3-1 mm and 25% of flotation magnesite with the thickness of 1-0 mm; 13% of 3-1 mm electric melting magnesia-alumina spinel and 5% of 1-0 mm electric melting magnesia-alumina spinel.
The preparation method of the flotation magnesite thermally mismatched toughened low-impurity magnesia-alumina spinel brick comprises the following steps:
c. weighing the raw materials according to the proportion, placing 5.4kg of the flotation magnesia particles and 1.8kg of the raw materials of the electric melting magnesia-alumina spinel particles in a powerful mixing roll to mix for 2 minutes, and then adding 220ml of water-soluble dextrin solution to mix for 4 minutes;
d. adding 2.8kg of high-purity magnesite fine powder serving as a fine powder raw material into the mixture a, and premixing for 15 minutes to obtain a mixed material;
c. b, adding the mixed material obtained in the step b into an assembled die, and pressing and forming by adopting a 630-ton press to obtain a green brick;
d. drying in a drying kiln for more than 24 hours, wherein the inlet temperature of the drying kiln is less than 70 ℃, and the highest drying temperature is controlled to be 110-130 ℃.
e. And (3) sintering in a box-type resistance furnace at 1650 ℃ for 4 hours at high temperature, wherein the total sintering time is 140-180 hours.
Example 3 (non-calcined alumina powder)
A flotation magnesite thermal mismatch toughened low-impurity magnesia-alumina spinel brick is prepared from the following components in percentage by weight and a water-soluble dextrin solution (the specific gravity is 1.2) accounting for 2.2 percent of the total weight of the following components:
54% of flotation magnesite with the MgO content of 97.63%, 18% of fused magnesia-alumina spinel and 28% of high-purity magnesite powder, wherein 7% of flotation magnesite with the thickness of 5-3 mm, 22% of flotation magnesite with the thickness of 3-1 mm and 25% of flotation magnesite with the thickness of 1-0 mm; 13% of 3-1 mm electric melting magnesia-alumina spinel and 5% of 1-0 mm electric melting magnesia-alumina spinel.
The preparation method of the flotation magnesite thermally mismatched toughened low-impurity magnesia-alumina spinel brick comprises the following steps:
a. weighing the raw materials according to the proportion, placing 5.4kg of the flotation magnesia particles and 1.8kg of the raw materials of the electric melting magnesia-alumina spinel particles in a powerful mixing roll to mix for 2 minutes, and then adding 220ml of water-soluble dextrin solution to mix for 4 minutes;
b. adding 2.8kg of high-purity magnesite fine powder serving as a fine powder raw material into the mixture a, and premixing for 15 minutes to obtain a mixed material;
c. b, adding the mixed material obtained in the step b into an assembled die, and pressing and forming by adopting a 630-ton press to obtain a green brick;
d. drying in a drying kiln for more than 24 hours, wherein the inlet temperature of the drying kiln is less than 70 ℃, and the highest drying temperature is controlled to be 110-130 ℃.
e. And (3) sintering in a box-type resistance furnace at 1700 ℃, keeping the temperature at high temperature for 4 hours, and keeping the total sintering time at 140-180 hours.
Example 4 (non-calcined alumina powder)
A flotation magnesite thermal mismatch toughened low-impurity magnesia-alumina spinel brick is prepared from the following components in percentage by weight and a water-soluble dextrin solution (the specific gravity is 1.2) accounting for 2.2 percent of the total weight of the following components:
57% of flotation magnesite with the MgO content of 97.63%, 15% of electric melting magnesia-alumina spinel and 28% of high-purity magnesite powder, wherein 7% of flotation magnesite with the thickness of 5-3 mm, 22% of flotation magnesite with the thickness of 3-1 mm and 28% of flotation magnesite with the thickness of 1-0 mm; 13% of 3-1 mm electric melting magnesia-alumina spinel and 2% of 1-0 mm electric melting magnesia-alumina spinel.
The preparation method of the flotation magnesite thermally mismatched toughened low-impurity magnesia-alumina spinel brick comprises the following steps:
a. weighing the raw materials according to the proportion, placing 5.7kg of the flotation magnesia particles and 1.5kg of the raw materials of the electric melting magnesia-alumina spinel particles in a powerful mixing roll to mix for 2 minutes, and then adding 220ml of water-soluble dextrin solution to mix for 4 minutes;
b. adding 2.8kg of high-purity magnesite fine powder serving as a fine powder raw material into the mixture a, and premixing for 15 minutes to obtain a mixed material;
c. b, adding the mixed material obtained in the step b into an assembled die, and pressing and forming by adopting a 630-ton press to obtain a green brick;
d. drying in a drying kiln for more than 24 hours, wherein the inlet temperature of the drying kiln is less than 70 ℃, and the highest drying temperature is controlled to be 110-130 ℃.
e. And (3) sintering in a box-type resistance furnace at 1650 ℃ for 4 hours at high temperature, wherein the total sintering time is 140-180 hours.
Example 5 (non-calcined alumina powder)
A flotation magnesite thermal mismatch toughened low-impurity magnesia-alumina spinel brick is prepared from the following components in percentage by weight and a water-soluble dextrin solution (the specific gravity is 1.2) accounting for 2.2 percent of the total weight of the following components:
60% of flotation magnesite with the MgO content of 97.63%, 12% of fused magnesia-alumina spinel and 28% of high-purity magnesite powder, wherein 7% of flotation magnesite with the thickness of 5-3 mm, 28% of flotation magnesite with the thickness of 3-1 mm and 25% of flotation magnesite with the thickness of 1-0 mm; 7% of 3-1 mm fused magnesia-alumina spinel and 5% of 1-0 mm fused magnesia-alumina spinel.
The preparation method of the flotation magnesite thermally mismatched toughened low-impurity magnesia-alumina spinel brick comprises the following steps:
a. weighing the raw materials according to the proportion, placing 6.0kg of the flotation magnesia particles and 1.2kg of the raw materials of the electric melting magnesia-alumina spinel particles in a powerful mixing roll to mix for 2 minutes, and then adding 220ml of water-soluble dextrin solution to mix for 4 minutes;
b. adding 2.8kg of high-purity magnesite fine powder serving as a fine powder raw material into the mixture a, and premixing for 15 minutes to obtain a mixed material;
c. b, adding the mixed material obtained in the step b into an assembled die, and pressing and forming by adopting a 630-ton press to obtain a green brick;
d. drying in a drying kiln for more than 24 hours, wherein the inlet temperature of the drying kiln is less than 70 ℃, and the highest drying temperature is controlled to be 110-130 ℃.
e. And (3) sintering in a box-type resistance furnace at 1650 ℃ for 4 hours at high temperature, wherein the total sintering time is 140-180 hours.
Example 6 (non-calcined alumina powder)
A flotation magnesite thermal mismatch toughened low-impurity magnesia-alumina spinel brick is prepared from the following components in percentage by weight and a water-soluble dextrin solution (the specific gravity is 1.2) accounting for 2.2 percent of the total weight of the following components:
50% of flotation magnesite with the MgO content of 97.63%, 22% of fused magnesia-alumina spinel and 28% of high-purity magnesite powder, wherein 7% of flotation magnesite with the thickness of 5-3 mm, 20% of flotation magnesite with the thickness of 3-1 mm and 23% of flotation magnesite with the thickness of 1-0 mm; 15% of 3-1 mm electric melting magnesia-alumina spinel and 7% of 1-0 mm electric melting magnesia-alumina spinel.
The preparation method of the flotation magnesite thermally mismatched toughened low-impurity magnesia-alumina spinel brick comprises the following steps:
a. weighing the raw materials according to the proportion, placing 5.0kg of the flotation magnesia particles and 2.2kg of the raw materials of the electric melting magnesia-alumina spinel particles in a powerful mixing roll to mix for 2 minutes, and then adding 220ml of water-soluble dextrin solution to mix for 4 minutes;
b. adding 2.8kg of high-purity magnesite fine powder serving as a fine powder raw material into the mixture a, and premixing for 15 minutes to obtain a mixed material;
c. b, adding the mixed material obtained in the step b into an assembled die, and pressing and forming by adopting a 630-ton press to obtain a green brick;
d. drying in a drying kiln for more than 24 hours, wherein the inlet temperature of the drying kiln is less than 70 ℃, and the highest drying temperature is controlled to be 110-130 ℃.
e. And (3) sintering in a box-type resistance furnace at 1650 ℃ for 4 hours at high temperature, wherein the total sintering time is 140-180 hours.
Example 7 (non-calcined alumina powder)
A flotation magnesite thermal mismatch toughened low-impurity magnesia-alumina spinel brick is prepared from the following components in percentage by weight and a water-soluble dextrin solution (the specific gravity is 1.2) accounting for 2.2 percent of the total weight of the following components:
59% of flotation magnesite with the MgO content of 97.63%, 13% of electric melting magnesia-alumina spinel and 28% of high-purity magnesite powder, wherein 7% of flotation magnesite with the thickness of 5-3 mm, 25% of flotation magnesite with the thickness of 3-1 mm and 27% of flotation magnesite with the thickness of 1-0 mm; 10% of 3-1 mm electric melting magnesia-alumina spinel and 3% of 1-0 mm electric melting magnesia-alumina spinel.
The preparation method of the flotation magnesite thermally mismatched toughened low-impurity magnesia-alumina spinel brick comprises the following steps:
a. weighing the raw materials according to the proportion, placing 5.9kg of the flotation magnesia particles and 1.3kg of the raw materials of the electric melting magnesia-alumina spinel particles in a powerful mixing roll to mix for 2 minutes, and then adding 220ml of water-soluble dextrin solution to mix for 4 minutes;
b. adding 2.8kg of high-purity magnesite fine powder serving as a fine powder raw material into the mixture a, and premixing for 15 minutes to obtain a mixed material;
c. b, adding the mixed material obtained in the step b into an assembled die, and pressing and forming by adopting a 630-ton press to obtain a green brick;
d. drying in a drying kiln for more than 24 hours, wherein the inlet temperature of the drying kiln is less than 70 ℃, and the highest drying temperature is controlled to be 110-130 ℃.
e. And (3) sintering in a box-type resistance furnace at 1650 ℃ for 4 hours at high temperature, wherein the total sintering time is 140-180 hours.
Example 8 (containing calcined alumina powder) (M3)
A flotation magnesite thermal mismatch toughened low-impurity magnesia-alumina spinel brick is prepared from the following components in percentage by weight and a water-soluble dextrin solution (the specific gravity is 1.2) accounting for 2.5 percent of the total weight of the following components:
54% of flotation magnesite with the MgO content of 97.63%, 18% of fused magnesia-alumina spinel, 26% of high-purity magnesite powder and 2% of calcined alumina micropowder, wherein 7% of 5-3 mm flotation magnesite, 22% of 3-1 mm flotation magnesite and 25% of 1-0 mm flotation magnesite are contained; 13% of 3-1 mm electric melting magnesia-alumina spinel and 5% of 1-0 mm electric melting magnesia-alumina spinel.
The preparation method of the flotation magnesite thermally mismatched toughened low-impurity magnesia-alumina spinel brick comprises the following steps:
a. weighing the raw materials according to the proportion, placing 5.4kg of the flotation magnesia particles and 1.8kg of the raw materials of the electric melting magnesia-alumina spinel particles in a powerful mixing roll to mix for 2 minutes, and then adding 230ml of water-soluble dextrin solution to mix for 4 minutes;
b. adding 2.6kg of high-purity magnesite fine powder serving as a fine powder raw material and 0.2kg of calcined alumina micro powder into the mixture a, and premixing for 15 minutes to obtain a mixed material;
c. b, adding the mixed material obtained in the step b into an assembled die, and pressing and forming by adopting a 630-ton press to obtain a green brick;
d. drying in a drying kiln for more than 24 hours, wherein the inlet temperature of the drying kiln is less than 70 ℃, and the highest drying temperature is controlled to be 110-130 ℃.
e. And (3) sintering in a box-type resistance furnace at 1650 ℃ for 4 hours at high temperature, wherein the total sintering time is 140-180 hours.
Example 9 (containing calcined alumina powder) (M4)
A flotation magnesite thermal mismatch toughened low-impurity magnesia-alumina spinel brick is prepared from the following components in percentage by weight and a water-soluble dextrin solution (the specific gravity is 1.2) accounting for 2.5 percent of the total weight of the following components:
54% of flotation magnesite with the MgO content of 97.63%, 18% of fused magnesia-alumina spinel, 23% of high-purity magnesite powder and 5% of calcined alumina micropowder, wherein 7% of 5-3 mm flotation magnesite, 22% of 3-1 mm flotation magnesite and 25% of 1-0 mm flotation magnesite are contained; 13% of 3-1 mm electric melting magnesia-alumina spinel and 5% of 1-0 mm electric melting magnesia-alumina spinel.
The preparation method of the flotation magnesite thermally mismatched toughened low-impurity magnesia-alumina spinel brick comprises the following steps:
a. weighing the raw materials according to the proportion, placing 5.4kg of the flotation magnesia particles and 1.8kg of the raw materials of the electric melting magnesia-alumina spinel particles in a powerful mixing roll to mix for 2 minutes, and then adding 230ml of water-soluble dextrin solution to mix for 4 minutes;
b. adding 2.3kg of high-purity magnesite fine powder and 0.5kg of calcined alumina micro powder serving as fine powder raw materials into the mixture a, and premixing for 15 minutes to obtain a mixed material;
c. b, adding the mixed material obtained in the step b into an assembled die, and pressing and forming by adopting a 630-ton press to obtain a green brick;
d. drying in a drying kiln for more than 24 hours, wherein the inlet temperature of the drying kiln is less than 70 ℃, and the highest drying temperature is controlled to be 110-130 ℃.
e. And (3) sintering in a box-type resistance furnace at 1650 ℃ for 4 hours at high temperature, wherein the total sintering time is 140-180 hours.
Example 10 (containing calcined alumina powder)
A flotation magnesite thermal mismatch toughened low-impurity magnesia-alumina spinel brick is prepared from the following components in percentage by weight and a water-soluble dextrin solution (the specific gravity is 1.2) accounting for 2.5 percent of the total weight of the following components:
54% of flotation magnesite with the MgO content of 97.63%, 18% of fused magnesia-alumina spinel, 19% of high-purity magnesite powder and 9% of calcined alumina micropowder, wherein 7% of 5-3 mm flotation magnesite, 22% of 3-1 mm flotation magnesite and 25% of 1-0 mm flotation magnesite are contained; 13% of 3-1 mm electric melting magnesia-alumina spinel and 5% of 1-0 mm electric melting magnesia-alumina spinel.
The preparation method of the flotation magnesite thermally mismatched toughened low-impurity magnesia-alumina spinel brick comprises the following steps:
a. weighing the raw materials according to the proportion, placing 5.4kg of the flotation magnesia particles and 1.8kg of the raw materials of the electric melting magnesia-alumina spinel particles in a powerful mixing roll to mix for 2 minutes, and then adding 230ml of water-soluble dextrin solution to mix for 4 minutes;
b. adding 1.9kg of high-purity magnesite fine powder and 0.9kg of calcined alumina micro powder which are used as fine powder raw materials into the mixture a, and premixing for 15 minutes to obtain a mixed material;
c. b, adding the mixed material obtained in the step b into an assembled die, and pressing and forming by adopting a 630-ton press to obtain a green brick;
d. drying in a drying kiln for more than 24 hours, wherein the inlet temperature of the drying kiln is less than 70 ℃, and the highest drying temperature is controlled to be 110-130 ℃.
e. And (3) sintering in a box-type resistance furnace at 1650 ℃ for 4 hours at high temperature, wherein the total sintering time is 140-180 hours.
Comparative example 1
The most common refractory product M1 (made of sintered magnesia as the main raw material) is currently commercially available.
Effect verification
1. The performance of the magnesia-alumina spinel brick obtained in the above example and the refractory material obtained in the comparative example were tested, and the results were as follows:
table 1 comparative test data
Figure BDA0002827429460000131
As can be seen from table 1:
(1) compared with the magnesia-alumina spinel brick M1, the magnesia-alumina spinel brick M2 prepared by adopting high-volume-density and high-purity flotation magnesia has the room-temperature compressive strength (meeting the industrial requirements)>55 MPa) and a smaller difference in softening temperature under load, M2 has a higher bulk density of 2.95g/cm3And a lower porosity of 16.6% (lower than the porosity of 17.1% of M1).
For refractory materials, small changes in porosity and bulk density values can have a significant effect on the performance of the product. Based on the test results, the sintering densification degree of the magnesia-alumina spinel brick is higher, and the penetration of aggressive substances can be effectively reduced.
(2) When calcining Al2O3When the addition amount of the fine powder is increased, the apparent porosity is reduced, the volume density is increased, and the M3 apparent porosity and the volume density are respectively 15 percent and 3.01g/cm3(ii) a Further increase, the apparent porosity of M4 was further reduced to 14.5%, and the bulk density was increased to 3.03g/cm3。
2. In order to further characterize the high-temperature performance of the material, water-cooling thermal shock tests were respectively carried out on M2, M3 and M4, and a magnesium aluminate spinel brick M1, and the appearance after thermal shock is shown in FIG. 2.
Wherein the water-cooling thermal shock frequency of the magnesia-alumina spinel brick M1 is 12 times, and the magnesia flotation magnesia prepared magnesia-alumina spinel brick M2 has lower SiO content2And the content of CaO impurities reduces the formation of low-temperature phases in the material, improves the thermal shock stability of the material, and the water-cooling thermal shock frequency is more than 25 times. With calcination of Al2O3The introduction amount of the fine powder is increased, the water-cooling thermal shock times of M3 and M4 are both more than 25, and the appearance is more complete after the thermal shock.
Further, Al is calcined2O3As the amount of the fine powder introduced increases, the porosity decreases and the powder becomes gradually dense, the high-temperature rupture strength increases and a certain high-temperature toughness is exhibited, as shown in fig. 1, it is seen that the brittle fracture is not direct but the stress impact is resisted within a certain period of time.
Calcination of Al in matrix for preparing magnesia-alumina spinel brick by using flotation magnesite2O3Introducing fine powder to form uniformly distributed in-situ magnesia-alumina spinel with magnesium oxide, and calcining Al2O3The content of the magnesia-alumina spinel is increased by the introduction amount of the fine powder. The spinel and periclase coefficients of thermal expansion in the matrix are mismatched when subjected to thermal shock (periclase 13.5X 10)-6K-1Spinel 8X 10-6K-1) Evenly distributed microcracks are formed, and the thermal shock stability and the high-temperature toughness of the material are improved.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. A magnesia-alumina spinel brick is characterized in that flotation magnesia, high-purity magnesia and electric melting magnesia-alumina spinel are used as main raw materials and are prepared by high-temperature treatment;
the mass ratio of the flotation magnesia to the high-purity magnesia to the fused magnesia-alumina spinel is (54-65): (18-28): (12-25).
2. The magnesia-alumina spinel brick of claim 1, wherein the mass ratio of the flotation magnesia to the high-purity magnesia to the electric melting magnesia-alumina spinel is (54-60): (19-28): (13-22);
and/or the main indexes of the flotation magnesite are as follows: the MgO content is 97.63%, SiO2The content is less than or equal to 0.5 percent, the CaO content is less than or equal to 1.0 percent, and the volume density is more than or equal to 3.3g/cm3The granularity is 200 meshes;
and/or the main indexes of the high-purity magnesite are as follows: al (Al)2O3The content is less than or equal to 0.1 percent, the content of MgO is more than or equal to 97 percent, and SiO2The content is less than or equal to 1.0 percent, the CaO content is less than or equal to 1.5 percent, and the granularity is 180 meshes;
and/or, the electricityThe main indexes of the fused magnesia-alumina spinel are as follows: al (Al)2O3The content is more than or equal to 65 percent, the content of CaO is less than or equal to 1.0 percent, the content of MgO is more than or equal to 30 percent, and the content of SiO is2The content is less than or equal to 0.5 percent, and the volume density is more than or equal to 3.3g/cm3。
3. The magnesia-alumina spinel brick of claim 2, wherein the particle size composition of the floated magnesite is controlled to be: 7% of flotation magnesite with the thickness of 5-3 mm, 22% of flotation magnesite with the thickness of 3-1 mm and 25% of flotation magnesite with the thickness of 1-0 mm;
and/or controlling the grain size composition of the fused magnesia-alumina spinel to be as follows: 13% of 3-1 mm electric melting magnesia-alumina spinel and 5% of 1-0 mm electric melting magnesia-alumina spinel.
4. The magnesia-alumina spinel brick of claim 3, wherein the raw materials comprise the following components in percentage by mass: 7-8% of flotation magnesite with the granularity of 5-3 mm, 20-28% of flotation magnesite with the granularity of 3-1 mm and 23-28% of flotation magnesite with the granularity of 1-0 mm; 7-13% of fused magnesia-alumina spinel with the granularity of 3-1 mm and 2-7% of fused magnesia-alumina spinel with the granularity of 1-0 mm.
5. The magnesia-alumina spinel brick of any one of claims 1 to 4, wherein the raw material further comprises calcined alumina powder in an amount of not more than 10% by mass of the total mass of the raw material.
6. The magnesia-alumina spinel brick of claim 5, wherein the mass ratio of the flotation magnesia to the high-purity magnesia to the fused magnesia-alumina spinel to the calcined alumina powder is (54-56): (19-26): (18-20): (2-9).
7. The magnesia-alumina spinel brick of claim 6, wherein the raw materials comprise the following components in percentage by mass: 7-8% of flotation magnesite with the granularity of 5-3 mm, 22-24% of flotation magnesite with the granularity of 3-1 mm and 25-28% of flotation magnesite with the granularity of 1-0 mm; 10-13% of fused magnesia-alumina spinel with the granularity of 3-1 mm and 5-7% of fused magnesia-alumina spinel with the granularity of 1-0 mm.
8. A method for preparing the magnesia-alumina spinel brick of any one of claims 1 to 7, which comprises the following steps: mixing the raw materials, pressing, drying and sintering;
wherein the mixing process comprises: mixing the floated magnesite and the fused magnesia-alumina spinel particles, and then mixing the mixture with a binding agent to form a mixture A; and mixing the high-purity magnesite with the mixture A to obtain a mixed material.
9. The preparation method according to claim 8, wherein the sintering temperature is controlled to be 1600-1700 ℃, the high temperature is kept constant for 3-4 hours, and the total sintering time is 140-180 hours;
and/or, the pressing is performed with a 630 ton or 1000 ton press;
and/or the drying temperature is controlled to be 110-130 ℃.
10. Use of the magnesia alumina spinel brick of any one of claims 1 to 7 in a refractory material.
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