CN108558378B - Alumina clinker with hierarchical pore structure and preparation method thereof - Google Patents

Alumina clinker with hierarchical pore structure and preparation method thereof Download PDF

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CN108558378B
CN108558378B CN201810748874.3A CN201810748874A CN108558378B CN 108558378 B CN108558378 B CN 108558378B CN 201810748874 A CN201810748874 A CN 201810748874A CN 108558378 B CN108558378 B CN 108558378B
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alumina
micro powder
pore structure
zirconium
nitrate
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CN108558378A (en
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顾华志
付绿平
黄奥
张美杰
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Wuhan University of Science and Engineering WUSE
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Abstract

The invention relates to a multistage pore structure alumina clinker and a preparation method thereof. The technical scheme is as follows: firstly, taking 85-93 wt% of bauxite raw material micro powder, 0.1-10 wt% of alumina micro powder, 0.1-5 wt% of silica micro powder and 0.1-8 wt% of soluble salt as raw materials, adding water accounting for 30-50 wt% of the raw materials, and uniformly mixing in a planetary ball mill to obtain a pug; then, forming the pug in a vacuum pug extruder to obtain a green body; and then drying the green body at 110-200 ℃ for 12-36 hours, and preserving heat at 1550-1750 ℃ for 1-8 hours to obtain the multistage pore structure alumina clinker. The method has low cost and simple process, and the prepared alumina clinker with the hierarchical pore structure contains micro-nano multilevel intracrystalline pores and has the characteristics of good mechanical property, good thermal shock resistance, low thermal conductivity and strong slag resistance.

Description

Alumina clinker with hierarchical pore structure and preparation method thereof
Technical Field
The invention belongs to the technical field of alumina clinker. In particular to alumina clinker with a hierarchical pore structure and a preparation method thereof.
Background
With the rapid development of economy, the demand of high energy consumption industries such as steel, cement, power industry and the like on energy sources is increasing day by day, and the contradiction between the shortage of energy sources and the rapid increase of the demand is highlighted day by day. The modern high-temperature industry not only requires the used refractory materials to have excellent mechanical strength, good heat peeling resistance, excellent erosion resistance and scouring resistance, but also requires low energy consumption and high thermal efficiency. Therefore, the development of high-quality refractories satisfying the above-mentioned various functions has been a major research focus in the refractory industry.
The reduction in weight of the working layer refractory is considered to be an effective way to realize a high-quality, multifunctional refractory. Firstly, the light weight can improve the heat insulation performance of a working layer and reduce heat dissipation, thereby reducing heat loss and heating cost and being beneficial to realizing energy conservation and emission reduction; secondly, air holes introduced in the light weight process can effectively accommodate thermal stress when the temperature changes sharply, and the heat peeling resistance of the refractory material of the working layer is favorably improved; finally, when the pore size of the prepared lightweight refractory material is small, the influence on the slag resistance and the mechanical strength of the refractory material is small, and even the influence can be improved.
However, the pores introduced during the weight reduction process affect the mechanical strength and slag resistance of the material, and therefore, the key to the weight reduction of the working layer refractory material is to provide reliable mechanical strength and slag resistance. Since weight reduction of refractory materials is generally achieved by preparing lightweight refractory aggregates, it is generally considered that lowering the apparent porosity and pore size of lightweight refractory materials is expected to achieve a balance between low thermal conductivity, high mechanical strength and reliable slag resistance.
In recent years, many studies on lightweight aggregates and their corresponding lightweight refractory materials for working linings have been conducted worldwide, and many methods for preparing lightweight aggregates have been reported, mainly by making holes by two means: (1) introducing some substance capable of occupying a certain space into the green body, and decomposing or discharging the substance through heat treatment to form pores, such as a pore-forming agent adding method, an in-situ decomposition method, a direct foaming method and the like. (2) Pores formed by particle packing in the green body are preserved inside the material by introducing additives or fine particles, such as particle packing method, reaction bonding method, etc. The former is a channel which is inevitably formed due to the decomposition and discharge of substances in the heat treatment process, and pores exist in the form of open pores; the latter mainly hinders the expulsion of the pores by reducing the diffusion rate during the sintering of the material; however, since diffusion is suppressed, the rate of movement of grain boundaries is also reduced, and pores inside the material are also mainly open pores.
In conclusion, the refractory aggregate prepared by the method has high apparent porosity and large pore diameter, and cannot resist the corrosion and the penetration of slag and high-temperature media in the using process.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a preparation method of alumina clinker with a multilevel pore structure, which has low cost and simple process; the alumina clinker with the hierarchical pore structure prepared by the method contains micro-nano multilevel intracrystalline pores, and has good mechanical property, good thermal shock resistance, low thermal conductivity and strong slag resistance.
In order to realize the task, the technical scheme adopted by the invention is as follows: firstly, taking 85-93 wt% of bauxite raw material micro powder, 0.1-10 wt% of alumina micro powder, 0.1-5 wt% of silica micro powder and 0.1-8 wt% of soluble salt as raw materials, adding 30-50 wt% of water to the raw materials, and uniformly mixing in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at 110-200 ℃ for 12-36 hours, and preserving heat at 1550-1750 ℃ for 1-8 hours to obtain the multistage pore structure bauxite clinker.
Al of the alumina raw material micro powder2O3Content is more than or equal to 45 wt%, and particle diameter D501 to 10 μm.
Al of the alumina micropowder2O3Content is more than or equal to 98 wt%, particle diameter D501 to 8 μm.
SiO of the fine silica powder2Content is more than or equal to 90 wt%, and particle diameter D500.1 to 3 μm.
The soluble salt is 1-4 of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
(1) according to the invention, soluble salt is introduced, and the soluble salt is hydrolyzed when being dissolved in water, so that hydrated cations can be formed, the hydrated cations exist in a tetramer or dimer form, and bridging hydroxyl groups of the hydrated cations can be connected with each other, thereby forming a network structure with nanopores in situ. The water and the alumina raw material micro powder introduced by the invention can form a micron pore structure in situ in the heat treatment process.
(2) In the heat treatment process, on one hand, the nano particles formed by decomposing the tetramer or dimer and the alumina raw material micro powder form staggered sintering, and due to the difference of sintering performances of the nano particles and the alumina raw material micro powder, in-situ stress is formed at the neck of the particles; on the other hand, the introduced alumina micro powder and silica micro powder can react with the alumina raw material micro powder, and the volume expansion in the reaction process forms in-situ stress in the material. The in-situ stress and the in-situ corresponding force can promote the high-temperature superplasticity of the nano particles to play, and the grain boundary moves rapidly, so that the micro and nano pores are rapidly sealed in the grains. In addition, the nano particles have larger surface diffusivity and surface energy, and can reduce the dividing and closing time of the intragranular pores, so that the intragranular pores are quickly divided into a large number of more tiny nanoscale pores, and a micro-nano multilevel intragranular pore structure is formed.
(3) Due to the micro-nano multilevel intra-crystalline pores, the heat conductivity coefficient of the alumina clinker with the multilevel pore structure can be reduced; secondly, the energy for reducing crack propagation can be absorbed, the cracks are bridged and deflected, and the mechanical property of the alumina clinker with the hierarchical pore structure is improved; and finally, when the material reacts with molten slag, supersaturation of a slag corrosion phase is facilitated, the growth rate of crystals is increased, an isolation layer is formed in situ, and the molten slag resistance of the alumina clinker with the hierarchical pore structure is improved.
The multistage pore structure alumina clinker prepared by the invention is detected as follows: the bulk density is 2.7 to 3.2g/cm3(ii) a The apparent porosity is 2-12%; the thermal conductivity coefficient at 800 ℃ is 2.3-4.0 W.m-1·K-1(ii) a The average pore diameter is 100 to 300 nm.
Therefore, the method has low cost and simple process, and the prepared alumina clinker with the hierarchical pore structure contains micro-nano hierarchical intragranular pores and has the characteristics of good mechanical property, good thermal shock resistance, low thermal conductivity and strong slag resistance.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting the scope of protection.
In order to avoid repetition, the raw materials related to this specific embodiment are uniformly described as follows, and are not described in detail in the embodiments:
al of the alumina raw material micro powder2O3Content is more than or equal to 45 wt%, and particle diameter D501 to 10 μm.
Al of the alumina micropowder2O3Content is more than or equal to 98 wt%, particle diameter D501 to 8 μm.
SiO of the fine silica powder2Content is more than or equal to 90 wt%, and particle diameter D500.1 to 3 μm.
Example 1
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, taking 85-87 wt% of bauxite raw material micro powder, 8.0-10 wt% of alumina micro powder, 2-5 wt% of silica micro powder and 2-4 wt% of soluble salt as raw materials, adding 30-40 wt% of water to the raw materials, and uniformly mixing in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1550-1650 ℃ for 4-8 hours to obtain the multi-level pore structure bauxite clinker.
The soluble salt is one of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate, and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 3.1-3.2 g/cm3(ii) a The apparent porosity is 2-6%; the thermal conductivity coefficient at 800 ℃ is 3.8-4.0 W.m-1·K-1(ii) a The average pore diameter is 100 to 200 nm.
Example 2
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, taking 85-87 wt% of bauxite raw material micro powder, 8.0-10 wt% of alumina micro powder, 2-5 wt% of silica micro powder and 2-4 wt% of soluble salt as raw materials, adding 30-40 wt% of water to the raw materials, and uniformly mixing in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1650-1750 ℃ for 1-5 hours to obtain the multistage pore structure bauxite clinker.
The soluble salt is a mixture of two of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 3.05-3.15 g/cm3(ii) a The apparent porosity is 3-7%; the thermal conductivity coefficient at 800 ℃ is 3.7-3.9 W.m-1·K-1(ii) a The average pore diameter is 100 to 200 nm.
Example 3
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, taking 85-87 wt% of bauxite raw material micro powder, 8.0-10 wt% of alumina micro powder, 2-5 wt% of silica micro powder and 2-4 wt% of soluble salt as raw materials, adding water accounting for 40-50 wt% of the raw materials, and uniformly mixing in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1550-1650 ℃ for 4-8 hours to obtain the multi-level pore structure bauxite clinker.
The soluble salt is a mixture of three substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 3.1-3.2 g/cm3(ii) a The apparent porosity is 3-8%; the thermal conductivity coefficient at 800 ℃ is 3.5-3.8 W.m-1·K-1(ii) a The average pore diameter is 100 to 200 nm.
Example 4
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, taking 85-87 wt% of bauxite raw material micro powder, 8.0-10 wt% of alumina micro powder, 2-5 wt% of silica micro powder and 2-4 wt% of soluble salt as raw materials, adding water accounting for 40-50 wt% of the raw materials, and uniformly mixing in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1650-1750 ℃ for 1-5 hours to obtain the multistage pore structure bauxite clinker.
The soluble salt is a mixture of four substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 3.1-3.2 g/cm3(ii) a The apparent porosity is 3-7%; the thermal conductivity coefficient at 800 ℃ is 3.6-3.8 W.m-1·K-1(ii) a The average pore diameter is 100 to 200 nm.
Example 5
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, taking 87-89 wt% of bauxite raw material micro powder, 5-8 wt% of alumina micro powder, 2-5 wt% of silica micro powder and 0.1-3 wt% of soluble salt as raw materials, adding 30-40 wt% of water to the raw materials, and uniformly mixing in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1550-1650 ℃ for 4-8 hours to obtain the multi-level pore structure bauxite clinker.
The soluble salt is one of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate, and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 3.1-3.2 g/cm3(ii) a The apparent porosity is 5-8%; the thermal conductivity coefficient at 800 ℃ is 3.1-3.4 W.m-1·K-1(ii) a The average pore diameter is 150 to 250 nm.
Example 6
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, taking 87-89 wt% of bauxite raw material micro powder, 5-8 wt% of alumina micro powder, 2-5 wt% of silica micro powder and 0.1-3 wt% of soluble salt as raw materials, adding 30-40 wt% of water to the raw materials, and uniformly mixing in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1650-1750 ℃ for 1-5 hours to obtain the multistage pore structure bauxite clinker.
The soluble salt is a mixture of two of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 3.0 to 3.1g/cm3(ii) a The apparent porosity is 4-7%; the thermal conductivity coefficient at 800 ℃ is 3.3-3.6 W.m-1·K-1(ii) a The average pore diameter is 150 to 300 nm.
Example 7
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, taking 87-89 wt% of bauxite raw material micro powder, 5-8 wt% of alumina micro powder, 2-5 wt% of silica micro powder and 0.1-3 wt% of soluble salt as raw materials, adding water accounting for 40-50 wt% of the raw materials, and uniformly mixing in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1550-1650 ℃ for 4-8 hours to obtain the multi-level pore structure bauxite clinker.
The soluble salt is a mixture of three substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 3.0 to 3.15g/cm3(ii) a The apparent porosity is 5-9%; the thermal conductivity coefficient at 800 ℃ is 3.2-3.5 W.m-1·K-1(ii) a The average pore diameter is 150 to 250 nm.
Example 8
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, taking 87-89 wt% of bauxite raw material micro powder, 5-8 wt% of alumina micro powder, 2-5 wt% of silica micro powder and 0.1-3 wt% of soluble salt as raw materials, adding water accounting for 40-50 wt% of the raw materials, and uniformly mixing in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1650-1750 ℃ for 1-5 hours to obtain the multistage pore structure bauxite clinker.
The soluble salt is a mixture of four substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 2.95-3.05 g/cm3(ii) a The apparent porosity is 5-8%; the thermal conductivity coefficient at 800 ℃ is 3.4-3.7 W.m-1·K-1(ii) a The average pore diameter is 150 to 250 nm.
Example 9
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, 89-91 wt% of bauxite raw material micro powder, 3-5 wt% of alumina micro powder, 0.1-3 wt% of silica micro powder and 3-5 wt% of soluble salt are used as raw materials, water accounting for 30-40 wt% of the raw materials is added, and the raw materials are uniformly mixed in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1550-1650 ℃ for 4-8 hours to obtain the multi-level pore structure bauxite clinker.
The soluble salt is one of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate, and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 2.85-3.05 g/cm3(ii) a The apparent porosity is 7-11%; the thermal conductivity coefficient at 800 ℃ is 2.7-2.9 W.m-1·K-1(ii) a The average pore diameter is 200 to 300 nm.
Example 10
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, 89-91 wt% of bauxite raw material micro powder, 3-5 wt% of alumina micro powder, 0.1-3 wt% of silica micro powder and 3-5 wt% of soluble salt are used as raw materials, water accounting for 30-40 wt% of the raw materials is added, and the raw materials are uniformly mixed in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1650-1750 ℃ for 1-5 hours to obtain the multistage pore structure bauxite clinker.
The soluble salt is a mixture of two of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 2.85-3.1 g/cm3(ii) a The apparent porosity is 7-10%; the thermal conductivity coefficient at 800 ℃ is 2.8-3.0 W.m-1·K-1(ii) a The average pore diameter is 150 to 250 nm.
Example 11
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, 89-91 wt% of bauxite raw material micro powder, 3-5 wt% of alumina micro powder, 0.1-3 wt% of silica micro powder and 3-5 wt% of soluble salt are used as raw materials, water accounting for 40-50 wt% of the raw materials is added, and the raw materials are uniformly mixed in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1550-1650 ℃ for 4-8 hours to obtain the multi-level pore structure bauxite clinker.
The soluble salt is a mixture of three substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 2.95-3.15 g/cm3(ii) a Air displayThe porosity is 6-10%; the thermal conductivity coefficient at 800 ℃ is 2.9-3.2 W.m-1·K-1(ii) a The average pore diameter is 150 to 250 nm.
Example 12
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, 89-91 wt% of bauxite raw material micro powder, 3-5 wt% of alumina micro powder, 0.1-3 wt% of silica micro powder and 3-5 wt% of soluble salt are used as raw materials, water accounting for 40-50 wt% of the raw materials is added, and the raw materials are uniformly mixed in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1650-1750 ℃ for 1-5 hours to obtain the multistage pore structure bauxite clinker.
The soluble salt is a mixture of four substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 3.0 to 3.15g/cm3(ii) a The apparent porosity is 7-9%; the thermal conductivity coefficient at 800 ℃ is 3.0-3.3 W.m-1·K-1(ii) a The average pore diameter is 200 to 300 nm.
Example 13
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, uniformly mixing 91-93 wt% of bauxite raw material micro powder, 0.1-3 wt% of alumina micro powder, 0.1-3 wt% of silica micro powder and 4-8 wt% of soluble salt serving as raw materials with water accounting for 30-40 wt% of the raw materials in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1550-1650 ℃ for 4-8 hours to obtain the multi-level pore structure bauxite clinker.
The soluble salt is one of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate, and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 2.7-2.95 g/cm3(ii) a The apparent porosity is 7-11%; the thermal conductivity coefficient at 800 ℃ is 2.3-2.5 W.m-1·K-1(ii) a The average pore diameter is 150 to 250 nm.
Example 14
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, uniformly mixing 91-93 wt% of bauxite raw material micro powder, 0.1-3 wt% of alumina micro powder, 0.1-3 wt% of silica micro powder and 4-8 wt% of soluble salt serving as raw materials with water accounting for 30-40 wt% of the raw materials in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1650-1750 ℃ for 1-5 hours to obtain the multistage pore structure bauxite clinker.
The soluble salt is a mixture of two of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 2.75-2.9 g/cm3(ii) a The apparent porosity is 8-12%; the thermal conductivity coefficient at 800 ℃ is 2.4-2.6 W.m-1·K-1(ii) a The average pore diameter is 150 to 250 nm.
Example 15
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, uniformly mixing 91-93 wt% of bauxite raw material micro powder, 0.1-3 wt% of alumina micro powder, 0.1-3 wt% of silica micro powder and 4-8 wt% of soluble salt serving as raw materials with water accounting for 40-50 wt% of the raw materials in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1550-1650 ℃ for 4-8 hours to obtain the multi-level pore structure bauxite clinker.
The soluble salt is a mixture of three substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 2.9-3.15 g/cm3(ii) a The apparent porosity is 7-12%; the heat conductivity coefficient at 800 ℃ is 2.6-2.8 W.m-1·K-1(ii) a The average pore diameter is 200 to 300 nm.
Example 16
A multi-level pore structure alumina clinker and a preparation method thereof. Firstly, uniformly mixing 91-93 wt% of bauxite raw material micro powder, 0.1-3 wt% of alumina micro powder, 0.1-3 wt% of silica micro powder and 4-8 wt% of soluble salt serving as raw materials with water accounting for 40-50 wt% of the raw materials in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; and drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1650-1750 ℃ for 1-5 hours to obtain the multistage pore structure bauxite clinker.
The soluble salt is a mixture of four substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The multistage pore structure alumina clinker prepared in the embodiment is detected as follows: the bulk density is 2.8-3.1 g/cm3(ii) a The apparent porosity is 7-11%; the thermal conductivity coefficient at 800 ℃ is 2.5-2.7 W.m-1·K-1(ii) a The average pore diameter is 200 to 300 nm.
Compared with the prior art, the specific implementation mode has the following positive effects:
(1) the soluble salt is introduced, and is hydrolyzed when being dissolved in water, so that hydrated cations can be formed, exist in a tetramer or dimer form, and bridging hydroxyl groups of the hydrated cations can be connected with each other, so that a network structure with nanopores is formed in situ. The water and the alumina raw material micro powder introduced by the embodiment can form a micron pore structure in situ in the heat treatment process.
(2) In the heat treatment process of the embodiment, on one hand, the nano particles formed by decomposing the tetramer or dimer and the alumina raw material micro powder form staggered sintering, and due to the difference of sintering performances of the nano particles and the alumina raw material micro powder, in-situ stress is formed at the neck part of the particles; on the other hand, the introduced alumina micro powder and silica micro powder can react with the alumina raw material micro powder, and the volume expansion in the reaction process forms in-situ stress in the material. The in-situ stress and the in-situ corresponding force can promote the high-temperature superplasticity of the nano particles to play, and the grain boundary moves rapidly, so that the micro and nano pores are rapidly sealed in the grains. In addition, the nano particles have larger surface diffusivity and surface energy, and can reduce the dividing and closing time of the intragranular pores, so that the intragranular pores are quickly divided into a large number of more tiny nanoscale pores, and a micro-nano multilevel intragranular pore structure is formed.
(3) Due to the micro-nano multilevel intra-crystalline pores, the heat conductivity coefficient of the alumina clinker with the multilevel pore structure can be reduced; secondly, the energy for reducing crack propagation can be absorbed, the cracks are bridged and deflected, and the mechanical property of the alumina clinker with the hierarchical pore structure is improved; and finally, when the material reacts with molten slag, supersaturation of a slag corrosion phase is facilitated, the growth rate of crystals is increased, an isolation layer is formed in situ, and the molten slag resistance of the alumina clinker with the hierarchical pore structure is improved.
The multistage pore structure alumina clinker prepared by the embodiment is detected as follows: the bulk density is 2.7 to 3.2g/cm3(ii) a The apparent porosity is 2-12%; the thermal conductivity coefficient at 800 ℃ is 2.3-4.0 W.m-1·K-1(ii) a The average pore diameter is 100 to 300 nm.
Therefore, the embodiment has low cost and simple process, and the prepared alumina clinker with the hierarchical pore structure contains micro-nano hierarchical intragranular pores and has the characteristics of good mechanical property, good thermal shock resistance, low thermal conductivity and strong slag resistance.

Claims (2)

1. The preparation method of the alumina clinker with the hierarchical pore structure is characterized by comprising the following steps of taking 85-93 wt% of alumina raw material micro powder, 0.1-10 wt% of alumina micro powder, 0.1-5 wt% of silica micro powder and 0.1-8 wt% of soluble salt as raw materials, adding 30-50 wt% of water to the raw materials, and uniformly mixing the raw materials in a planetary ball mill to obtain a mud material; then, forming the pug in a vacuum pug extruder to obtain a green body; drying the green body at 110-200 ℃ for 12-36 hours, and preserving heat at 1550-1750 ℃ for 1-8 hours to obtain the alumina clinker with the hierarchical pore structure;
al of the alumina raw material micro powder2O3Content is more than or equal to 45 wt%, and particle diameter D501 to 10 μm;
al of the alumina micropowder2O3Content is more than or equal to 98 wt%, particle diameter D501-8 μm;
SiO of the fine silica powder2Content is more than or equal to 90 wt%, and particle diameter D500.1 to 3 μm;
the soluble salt is 1-4 of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
2. A multi-pore-structure alumina clinker characterized in that the multi-pore-structure alumina clinker is prepared by the method for preparing a multi-pore-structure alumina clinker according to claim 1.
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