CN113480301B - Preparation method of large brick at bottom of high-temperature sillimanite pool of large float glass melting furnace - Google Patents

Preparation method of large brick at bottom of high-temperature sillimanite pool of large float glass melting furnace Download PDF

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CN113480301B
CN113480301B CN202110802792.4A CN202110802792A CN113480301B CN 113480301 B CN113480301 B CN 113480301B CN 202110802792 A CN202110802792 A CN 202110802792A CN 113480301 B CN113480301 B CN 113480301B
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sillimanite
temperature
hours
melting furnace
brick
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CN113480301A (en
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马乃甫
谭启煜
马晓东
翟所鹏
王德宏
翟所春
王光胜
张廷胜
张宗键
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Shandong Zibo Shenzi Refractory Materials Co ltd
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Shandong Zibo Shenzi Refractory Materials Co ltd
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    • 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
    • C04B35/16—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 silicates other than clay
    • C04B35/18—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 silicates other than clay rich in aluminium oxide
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Abstract

The invention belongs to the technical field of preparation of refractory materials, and particularly relates to a preparation method of a large brick at the bottom of a high-temperature sillimanite pool of a large float glass melting furnace. The preparation method comprises the steps of grading and selecting sillimanite, mixing raw materials, pouring and blank making, exhausting, demoulding, drying and high-temperature calcining. The high-temperature sillimanite pool bottom large brick prepared by the method uses natural mineral sillimanite as a main material, has a compact fine grain structure, is not easy to generate bubbles in the glass production process, completes secondary mullite formation to form compact crystals in the high-temperature calcination process for about 28 days, does not generate crystal expansion in the actual use process, keeps good high-temperature volume stability, is used at the bottom of a large float glass kiln, ensures the overall stability of a kiln body, improves the overall thermal efficiency of a melting furnace while ensuring enough high bearing capacity, and saves fuel cost.

Description

Preparation method of large brick at bottom of high-temperature sillimanite pool of large float glass melting furnace
Technical Field
The invention belongs to the technical field of preparation of refractory materials, and particularly relates to a preparation method of a large brick at the bottom of a high-temperature sillimanite pool of a large float glass melting furnace.
Background
With the leap development of glass production technology, the glass melting furnace is continuously developed as the core thermal equipment for glass production in the direction of higher efficiency and lower energy consumption, and the melting furnace is required to improve combustion intensity, strengthen heat radiation, enhance heat efficiency, reduce heat loss and reduce environmental pollution, so that the refractory material for building the melting furnace needs to bear higher temperature, more rapid temperature change, stronger chemical erosion and severe stress damage.
The glass melting furnace is a thermal equipment for melting glass, which is formed by scientifically preparing various refractory materials without reaction. As the physical, chemical and mechanical conditions of each part are different, the parts require the performance of the refractory material for the glass melting furnace to be suitable for the parts, and simultaneously, the parts do not have adverse effects on various adjacent refractory materials of other types so as to ensure that the melting furnace has long enough service life. The main task is to provide glass of the desired quality under conditions that are as economical as possible. With the increase of the application of various special glass in daily life, glass manufacturers require that newly-built glass melting furnaces have higher melting temperature, longer melting time and larger capacity of the melting furnaces, and the existing clay bricks at the bottom of the melting furnaces only have the supporting capability of a common melting furnace main body and the capability of resisting glass liquid erosion to a certain degree, and the requirements on larger melting furnace weight and higher temperature can not be met gradually.
Therefore, it is highly desirable to develop a large bottom brick suitable for a large float glass furnace.
Disclosure of Invention
The purpose of the invention is: provides a preparation method of a large brick at the bottom of a high-temperature sillimanite pool of a large float glass melting furnace. The large brick at the bottom of the pool prepared by the method is high temperature resistant; the electric melting paving brick is resistant to molten glass erosion, even if the electric melting paving brick contacting the molten glass is eroded and penetrated by the molten glass, the electric melting paving brick can be used continuously and checked in time, and sudden production accidents caused by the penetration of a kiln bottom are avoided; has enough supporting strength, and obviously improves the melting temperature and the thermal efficiency of the melting furnace.
The invention relates to a preparation method of a large brick at the bottom of a high-temperature sillimanite pool of a large float glass melting furnace, which comprises the following steps:
(1) Grading and selecting sillimanite: removing defective ores from natural sillimanite, then crushing and screening into different granularities, and performing strong magnetic iron removal;
(2) Mixing sillimanite, synthetic mullite, refractory clay, mullite fine powder, lignin and high-alumina cement according to a certain mass ratio, stirring for 20-30 minutes, and removing iron by strong magnetism again after grinding;
(3) Pouring and blank making: mixing the powder prepared in the step (2), the micro silicon powder, the paper pulp and water, pouring the mixture into a mold horizontally placed on a vibration platform, and performing high-frequency vibration molding to obtain a blank body;
(4) Exhausting: after the vibration is finished, the lower vibration platform is lifted together with the die, and a handheld vibrator is used for adhering the side wall of the die to move in a Z shape to perform cross exhaust;
(5) Demolding and drying: standing the blank together with the mold for 16-24 hours, demolding, naturally curing for a period of time after demolding, and then placing into a drying chamber for drying;
(6) High-temperature calcination: and (3) putting the blank dried in the step (5) into a high-temperature kiln, heating to 100-110 ℃ within 10-12 hours, keeping the temperature for 24-40 hours, heating to 500-505 ℃ within 40-80 hours, keeping the temperature for 12-24 hours, heating to 900-910 ℃ within 72-100 hours, keeping the temperature for 24-48 hours, heating to 1200-1205 ℃ within 90-160 hours, keeping the temperature for 20-30 hours, heating to 1520-1525 ℃ within 75-95 hours, keeping the temperature for 15-18 hours, cooling to 105-110 ℃ within 36-72 hours, opening the kiln, cooling, and performing post-treatment to obtain the large-scale float glass melting kiln high-temperature sillimanite pool bottom large brick.
Wherein:
after the natural sillimanite raw material in the step (1) is put into a factory, defective ores with more dark color impurities are firstly checked and sorted by naked eyes, crushed, carefully selected and screened into three particle size grades, wherein 0.5-1mm accounts for 8-12%,1-3mm accounts for 18-22%, and 3-5mm accounts for 68-72% in percentage by weight, and iron is removed by strong magnetism before the natural sillimanite raw material is put into different bins.
Preferably, after the natural sillimanite raw material in the step (1) enters a factory, defective ores with more dark color impurities are firstly checked and sorted by naked eyes, crushed, carefully selected and screened into three granularity grades, wherein the three granularity grades comprise 0.5-1mm, 1-3mm and 3-5mm in percentage by weight, and iron is removed by strong magnetism before the natural sillimanite raw material is distributed into different bins.
The sum of the mass of the sillimanite, the synthetic mullite, the refractory clay, the mullite fine powder, the lignin and the high alumina cement in the step (2) is 100 percent; wherein: 50-70% of sillimanite, 10-20% of synthetic mullite, 10-15% of refractory clay, 5-10% of mullite fine powder, 3-5% of lignin and 1-5% of high alumina cement.
And (3) putting the mixture into a powerful double-shaft stirrer to be stirred for 20-30 minutes, fully mixing other raw materials with the refractory clay, rubbing and grinding the mixture to fully and effectively infiltrate the refractory clay onto the surface of the mineral particles, and removing iron by strong magnetism again after grinding.
The sillimanite comprises the following chemical components: siO 2 2 35-38％、Al 2 O 3 58-60％、Fe 2 O 3 0.5-1.0％。
The refractory clay comprises the following chemical components: 46-51% of Al 2 O 3 39-42％，Fe 2 O 3 1.5-2.5％。
The granularity of the mullite fine powder is 0.5-1.5mm.
The high-alumina cement is CA50-A600.
The micro silicon powder comprises the following chemical components: siO 2 2 75-95％、Al 2 O 3 0.8-1.1％、Fe 2 O 3 0.6-0.9％、MgO 0.6-0.8％、CaO 0.2-0.4％、Na 2 1.1 to 1.2 percent of O; the granularity is 200 meshes.
The lignin is a commercial product.
The added micro silicon powder in the step (3) accounts for 1-3% of the powder prepared in the step (2) in mass.
The mass of the added water in the step (3) accounts for 5-10% of the powder prepared in the step (2).
The mass of the added paper pulp in the step (3) accounts for 1-3% of the powder prepared in the step (2).
The high-frequency vibration frequency in the step (3) is 80-100 times/min, and the time is less than 40min.
The size of the mould in the step (3) is as follows: the length is 1200-5000mm, the width is 800-2000mm, and the height is 500-1000mm.
The times of the cross air exhaust in the step (4) are 4-6 times, and the air exhaust process is completed within 3 minutes so as to avoid influencing the solidification of the embryo body.
The natural curing temperature in the step (5) is 15-30 ℃, and the time is 24-48h; the drying temperature is 45-65 ℃, the drying aims to fully remove internal free water and avoid internal cracking and line breaking of the embryo body in the calcining process.
And (4) the post-treatment in the step (6) is to cut the brick into proper size and shape according to the design requirement of the melting furnace, and polish six surfaces of the large brick at the bottom of the tank to be smooth, wherein the size tolerance is controlled to be between +0mm and-1 mm.
The sillimanite is transformed into a mullite phase at a high temperature of more than 1350 ℃, and the mullite phase is fixed in the continuous constant temperature process to avoid expansion and cracking of a brick body caused by secondary mullite in the use process. The higher the mullite degree is, the better the temperature resistance and high-temperature stability of the product are. The synthetic mullite and the mullite fine powder are added to adjust the aluminum content, promote sillimanite to complete secondary mullite in the sintering process, and meet the index requirements by matching with the sillimanite. The refractory clay provides buffer for the expansion of sillimanite particles in the sintering process, the cracking of a brick body in the sintering process is avoided, and the high-alumina cement and the micro-silica powder play a role of a binder; lignin and pulp are both binders, which aid the refractory clay in binding the particles.
Because the brick body size is big, needs to roast stage by stage, fully burns through inner structure, makes it produce the chemical reaction change under different temperatures, stabilizes the brick body when low temperature and prevents that the brick material from rising temperature too fast the hydrone in the brick body from diffusing rapidly and can lead to the brick body fracture, and calcination when high temperature makes the sillimanite change and becomes the mullite phase, and constant temperature calcination is firm mullite, avoids the production of secondary mullite in the use.
The staged roasting ensures that the ceramic is more tightly combined, the threshing phenomenon is absolutely avoided in the process of processing, cutting and grinding according to the designed size, and even the complicated special-shaped size can be accurately processed. The expansion is uniform at high temperature in the using process, and the cracking is not easy to occur.
The high-temperature sillimanite pool bottom big brick prepared by the method is used for building the necessary melting furnace section bottom in the production process of high-end glass such as electronic glass, high-alumina glass, ultrathin glass, ultra-white glass, photovoltaic glass, daily glass and the like, the working surface can effectively isolate the erosion of molten glass, meanwhile, the temperature resistance is higher, the actual using temperature reaches 1600 ℃, the brick is used for a large melting furnace with the daily melting amount exceeding 1100 tons/day, the brick has enough supporting strength, meanwhile, the melting temperature and the heat efficiency of the melting furnace are obviously improved, glass manufacturers are helped to improve the glass quality, and the fuel cost is saved.
Compared with the prior art, the invention has the following beneficial effects:
(1) The large brick at the bottom of the high-temperature sillimanite pool prepared by the method uses natural mineral sillimanite as a main material, has a compact fine-grain structure, is not easy to generate bubbles in the glass production process, completes secondary mullite to form compact crystals in the high-temperature calcination process for about 28 days, does not generate crystal expansion in the actual use process, keeps good high-temperature volume stability, is used at the bottom of a large float glass kiln, ensures the overall stability of a kiln body, improves the overall thermal efficiency of a melting kiln while ensuring enough high bearing capacity, and saves the fuel cost.
(2) The high-temperature sillimanite pool bottom big brick, al, prepared by the method of the invention 2 O 3 Content is more than or equal to 60 percent, fe 2 O 3 The content of the (B) is less than or equal to 1.0 percent, and the volume density is more than or equal to 2.45g/cm 3 The apparent porosity is less than or equal to 18 percent, the normal temperature compressive strength is more than or equal to 65MPa, and the supporting strength per unit area is more than 650kg/cm 2 Refractoriness under load T 0.6 The load temperature of 0.2MPa is more than or equal to 1500 ℃, and the re-burning line change of 1400 ℃ X2H is-0.2-0.1%.
(3) The high-temperature sillimanite pool bottom large brick prepared by the method resists molten glass erosion, can be used continuously and checked in time even if the electric melting paving bricks contacting molten glass are eroded and penetrated by the molten glass, and avoids sudden production accidents caused by the penetration of a kiln bottom hole.
(4) The preparation method of the large brick at the bottom of the high-temperature sillimanite pool has the advantages of wide raw material source and easily controlled process parameters, and is suitable for industrialized popularization and production.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
The preparation method of the large brick at the bottom of the high-temperature sillimanite pool of the large float glass melting furnace in the embodiment 1 comprises the following steps:
(1) Grading and refining sillimanite: removing defective ores from natural sillimanite, then crushing and screening into different granularities, and performing strong magnetic iron removal;
(2) Mixing sillimanite, synthetic mullite, refractory clay, mullite fine powder, lignin and high-alumina cement according to a certain mass ratio, stirring for 20 minutes, and removing iron by strong magnetism again after grinding;
(3) Pouring and blank making: mixing the powder prepared in the step (2), micro silicon powder, paper pulp and water, pouring the mixture into a mold horizontally placed on a vibration platform, and performing high-frequency vibration molding to obtain a blank body;
(4) Exhausting: after the vibration is finished, the lower vibration platform is lifted together with the die, and a handheld vibrator is used for adhering the side wall of the die to move in a Z shape to perform cross exhaust;
(5) Demolding and drying: standing the blank together with the die for 24 hours, demoulding, naturally curing for a period of time after demoulding, and then placing into a drying chamber for drying;
(6) High-temperature calcination: and (3) placing the blank dried in the step (5) into a high-temperature kiln, continuously heating to 105 ℃ within 11 hours, keeping the temperature for 38 hours, continuously heating to 505 ℃ within 60 hours, keeping the temperature for 20 hours, continuously heating to 905 ℃ within 92 hours, keeping the temperature for 40 hours, heating to 1200 ℃ within 145 hours, keeping the temperature for 27 hours, heating to 1520 ℃ within 85 hours, keeping the temperature for 17 hours, finally gradually cooling to 110 ℃ within 58 hours, opening the kiln, cooling, and performing post-treatment to obtain the large-scale float glass melting furnace high-temperature sillimanite pool bottom large brick.
Wherein:
after the natural sillimanite raw material in the step (1) is put into a factory, defective ores with more dark color impurities are firstly checked and sorted by naked eyes, crushed, carefully selected and screened into three granularity grades, wherein 0.5-1mm accounts for 8%,1-3mm accounts for 20% and 3-5mm accounts for 72% in percentage by weight, and iron is removed by strong magnetism before the natural sillimanite raw material is distributed into different bins.
The sum of the mass of the sillimanite, the synthetic mullite, the refractory clay, the mullite fine powder, the lignin and the high alumina cement in the step (2) is 100 percent; wherein: 60% of sillimanite, 15% of synthetic mullite, 12% of refractory clay, 7% of mullite fine powder, 4% of lignin and 2% of high-alumina cement.
And (3) putting the mixture into a powerful double-shaft stirrer to be stirred for 20 minutes in the step (2), fully mixing other raw materials with the refractory clay, rubbing and grinding the mixture to fully and effectively soak the refractory clay on the surface of mineral particles, and removing iron by strong magnetism again after grinding.
The sillimanite comprises the following chemical components: siO 2 2 38％、Al 2 O 3 60％、Fe 2 O 3 0.5％。
The refractory clay comprises the following chemical components: siO 2 2 50％，Al 2 O 3 41％，Fe 2 O 3 1.7％。
The granularity of the mullite fine powder is 1.0mm.
The high-alumina cement is CA50-A600.
The micro silicon powder comprises the following chemical components: siO 2 2 95％、Al 2 O 3 1.0％、Fe 2 O 3 0.7％、MgO 0.6％、CaO 0.2％、Na 2 1.1% of O; the granularity is 200 meshes.
The lignin is a commercial product.
The mass of the added micro silicon powder in the step (3) accounts for 2% of the powder prepared in the step (2).
The mass of the added water in the step (3) accounts for 7% of the powder prepared in the step (2).
The mass of the added paper pulp in the step (3) accounts for 3% of the powder prepared in the step (2).
The high-frequency vibration frequency in the step (3) is 90 times/min, and the time is 33min.
The size of the mould in the step (3) is as follows: the length is 1200mm, the width is 800mm, and the height is 500mm.
The number of times of cross air exhaust in the step (4) is 5, and the air exhaust process is completed within 3 minutes so as to avoid influencing the solidification of the embryo body.
The natural curing temperature in the step (5) is 20 ℃, and the time is 32 hours; the drying temperature is 65 ℃, the drying aims to fully remove internal free water and avoid internal cracking and line breaking of the embryo body in the calcining process.
And (4) the post-treatment in the step (6) is to cut the brick into proper size and shape according to the design requirement of the melting furnace, and polish six surfaces of the large brick at the bottom of the tank to be smooth, wherein the size tolerance is controlled to be between +0mm and-1 mm.
Example 2
The preparation method of the large brick at the bottom of the high-temperature sillimanite pool of the large float glass melting furnace in the embodiment 2 comprises the following steps:
(1) Grading and refining sillimanite: removing defective ores from natural sillimanite, then crushing and screening into different granularities, and performing strong magnetic iron removal;
(2) Mixing sillimanite, synthetic mullite, refractory clay, mullite fine powder, lignin and high-alumina cement according to a certain mass ratio, stirring for 30 minutes, and removing iron by strong magnetism again after grinding;
(3) Pouring and blank making: mixing the powder prepared in the step (2), the micro silicon powder, the paper pulp and water, pouring the mixture into a mold horizontally placed on a vibration platform, and performing high-frequency vibration molding to obtain a blank body;
(4) Exhausting: after the vibration is finished, the lower vibration platform is lifted together with the die, and a handheld vibrator is used for adhering the side wall of the die to move in a Z shape to perform cross exhaust;
(5) Demolding and drying: standing the blank together with the die for 16 hours, demoulding, naturally curing for a period of time after demoulding, and then placing into a drying chamber for drying;
(6) High-temperature calcination: and (3) putting the blank dried in the step (5) into a high-temperature kiln, continuously heating to 100 ℃ within 10 hours, keeping the temperature for 27 hours, continuously heating to 500 ℃ within 53 hours, keeping the temperature for 19 hours, continuously heating to 910 ℃ within 87 hours, keeping the temperature for 36 hours, heating to 1205 ℃ within 104 hours, keeping the temperature for 23 hours, heating to 1520 ℃ within 81 hours, keeping the temperature for 16 hours, finally gradually cooling to 110 ℃ within 50 hours, opening the kiln, cooling, and performing post-treatment to obtain the large-scale float glass melting furnace high-temperature sillimanite pool bottom large brick.
Wherein:
after the natural sillimanite raw material in the step (1) is put into a factory, defective ores with more dark color impurities are firstly checked and sorted by naked eyes, crushed, carefully selected and screened into three granularity grades, wherein the three granularity grades comprise 0.5-1mm, 1-3mm and 3-5mm in percentage by weight, and iron is removed by strong magnetism before the raw material is distributed into different bins.
The sum of the mass of the sillimanite, the synthetic mullite, the refractory clay, the mullite fine powder, the lignin and the high alumina cement in the step (2) is 100 percent; wherein: 50% of sillimanite, 20% of synthetic mullite, 15% of refractory clay, 8% of mullite fine powder, 3% of lignin and 4% of high-alumina cement.
And (3) putting the mixture into a powerful double-shaft stirrer to be stirred for 30 minutes in the step (2), fully mixing other raw materials with the refractory clay, rubbing and grinding the mixture to fully and effectively soak the refractory clay on the surface of mineral particles, and removing iron by strong magnetism again after grinding.
The sillimanite comprises the following chemical components: siO 2 2 38％、Al 2 O 3 60％、Fe 2 O 3 0.5％。
The refractory clay comprises the following chemical components: siO 2 2 50％，Al 2 O 3 41％，Fe 2 O 3 1.7％。
The granularity of the mullite fine powder is 1.5mm.
The high-alumina cement is CA50-A600.
The micro silicon powder comprises the following chemical components: siO 2 2 95％、Al 2 O 3 1.0％、Fe 2 O 3 0.7％、MgO 0.6％、CaO 0.2％、Na 2 1.1% of O; the granularity is 200 meshes.
The lignin is a commercial product.
The mass of the added micro silicon powder in the step (3) accounts for 1% of the powder prepared in the step (2).
The mass of the added water in the step (3) accounts for 10% of the powder prepared in the step (2).
The mass of the added paper pulp in the step (3) accounts for 3% of the powder prepared in the step (2).
The high-frequency vibration frequency in the step (3) is 80 times/min, and the time is 38min.
The size of the mould in the step (3) is as follows: 3100mm in length, 1400mm in width and 750mm in height.
The number of times of cross air exhaust in the step (4) is 4, and the air exhaust process is completed within 3 minutes so as to avoid influencing the solidification of the embryo body.
The natural curing temperature in the step (5) is 30 ℃, and the time is 24 hours; the drying temperature is 65 ℃, the drying aims to fully remove internal free water and avoid internal cracking and line breaking of the embryo body in the calcining process.
And (6) cutting the large bricks into proper sizes and shapes according to the design requirements of the melting furnace, and polishing six surfaces of the large bricks at the bottom of the tank until the six surfaces are smooth, wherein the dimensional tolerance is controlled to be +0 mm-1 mm.
Example 3
The preparation method of the large brick at the bottom of the high-temperature sillimanite pool of the large float glass melting furnace in the embodiment 3 comprises the following steps:
(1) Grading and refining sillimanite: removing defective ores from natural sillimanite, then crushing and screening into different granularities, and performing strong magnetic iron removal;
(2) Mixing sillimanite, synthetic mullite, refractory clay, mullite fine powder, lignin and high-alumina cement according to a certain mass ratio, stirring for 30 minutes, and removing iron by strong magnetism again after grinding;
(3) Pouring and blank making: mixing the powder prepared in the step (2), the micro silicon powder, the paper pulp and water, pouring the mixture into a mold horizontally placed on a vibration platform, and performing high-frequency vibration molding to obtain a blank body;
(4) Exhausting: after the vibration is finished, the lower vibration platform is lifted together with the die, and a handheld vibrator is used for adhering the side wall of the die to move in a Z shape to perform cross exhaust;
(5) Demolding and drying: standing the blank together with the die for 20 hours, demoulding, naturally curing for a period of time after demoulding, and then putting into a drying chamber for drying;
(6) High-temperature calcination: and (3) placing the blank dried in the step (5) into a high-temperature kiln, continuously heating to 110 ℃ within 12 hours, keeping the temperature for 40 hours, continuously heating to 500 ℃ within 80 hours, keeping the temperature for 24 hours, continuously heating to 900 ℃ within 100 hours, keeping the temperature for 48 hours, heating to 1200 ℃ within 160 hours, keeping the temperature for 30 hours, heating to 1520 ℃ within 95 hours, keeping the temperature for 18 hours, finally gradually cooling to 110 ℃ within 72 hours, opening the kiln, cooling, and performing post-treatment to obtain the large-scale float glass melting kiln high-temperature sillimanite pool bottom large brick.
Wherein:
after the natural sillimanite raw material in the step (1) is put into a factory, defective ores with more dark color impurities are firstly checked and sorted by naked eyes, crushed, carefully selected and screened into three granularity grades, wherein the three granularity grades comprise 0.5-1mm, 1-3mm and 3-5mm in percentage by weight, and iron is removed by strong magnetism before the raw material is distributed into different bins.
The sum of the mass of the sillimanite, the synthetic mullite, the refractory clay, the mullite fine powder, the lignin and the high alumina cement in the step (2) is 100 percent; wherein: 68% of sillimanite, 10% of synthetic mullite, 10% of refractory clay, 5% of mullite fine powder, 5% of lignin and 2% of high alumina cement.
And (3) putting the mixture into a powerful double-shaft stirrer to be stirred for 30 minutes in the step (2), fully mixing other raw materials with the refractory clay, rubbing and grinding the mixture to fully and effectively soak the refractory clay on the surface of mineral particles, and removing iron by strong magnetism again after grinding.
The sillimanite comprises the following chemical components: siO 2 2 38％、Al 2 O 3 60％、Fe 2 O 3 0.5％。
The refractory clay comprises the following chemical components: siO 2 2 50％，Al 2 O 3 41％，Fe 2 O 3 1.7％。
The granularity of the mullite fine powder is 0.5mm.
The high-alumina cement is CA50-A600.
The micro silicon powder comprises the following chemical components: siO 2 2 95％、Al 2 O 3 1.0％、Fe 2 O 3 0.7％、MgO 0.6％、CaO 0.2％、Na 2 1.1% of O; the granularity is 200 meshes.
The lignin is a commercial product.
The added micro silicon powder in the step (3) accounts for 3% of the powder prepared in the step (2).
The mass of the added water in the step (3) accounts for 8% of the powder prepared in the step (2).
The mass of the added paper pulp in the step (3) accounts for 2 percent of the powder prepared in the step (2).
The high-frequency vibration frequency in the step (3) is 100 times/min, and the time is 30min.
The size of the mould in the step (3) is as follows: 5000mm long, 2000mm wide and 1000mm high.
The number of times of cross air exhaust in the step (4) is 6, and the air exhaust process is completed within 3 minutes so as to avoid influencing the solidification of the embryo body.
The natural curing temperature in the step (5) is 25 ℃, and the time is 30 hours; the drying temperature is 60 ℃, the drying aims to fully remove internal free water and avoid internal cracking and line breaking of the embryo body in the calcining process.
And (6) cutting the large bricks into proper sizes and shapes according to the design requirements of the melting furnace, and polishing six surfaces of the large bricks at the bottom of the tank until the six surfaces are smooth, wherein the dimensional tolerance is controlled to be +0 mm-1 mm.
Comparative example 1
The preparation method of the glass melting furnace high-temperature sillimanite pool bottom big brick in the comparative example 1 is the same as that in the example 3, the only difference is that the high-temperature calcination step is different, and the high-temperature calcination in the comparative example 3 is as follows: and (4) putting the blank dried in the step (5) into a high-temperature kiln, heating to 1520 ℃ at a heating rate of 9.5 ℃/h, keeping the temperature for 447 hours, finally gradually cooling to 110 ℃ within 72 hours, opening the kiln, cooling, and performing post-treatment to obtain the large brick at the bottom of the high-temperature sillimanite pool of the large-scale float glass melting kiln.
The performance test of the high-temperature sillimanite pool bottom bricks prepared in examples 1 to 3 and comparative example 1 was carried out, and the results are shown in table 1 below.
TABLE 1 Large-scale float glass furnace high-temperature sillimanite pool bottom big brick performance detection index
Figure BDA0003165338880000081
Figure BDA0003165338880000091
The volume density and the apparent porosity are measured by GB/T2997-2015 test methods for the volume density, the apparent porosity and the true porosity of the dense-shaped refractory product; the normal temperature compressive strength is measured by a test method of the normal temperature compressive strength of a GB/T5072-2008 refractory material.
Of course, the foregoing is only a preferred embodiment of the invention and should not be taken as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit and scope of the present invention should be construed as being included in the scope of the present invention.

Claims (8)

1. A preparation method of a large brick at the bottom of a high-temperature sillimanite pool of a large float glass melting furnace is characterized by comprising the following steps: the method comprises the following steps:
(1) Grading and refining sillimanite: removing defective ores from natural sillimanite, then crushing and screening into different granularities, and performing strong magnetic iron removal;
(2) Mixing sillimanite, synthetic mullite, refractory clay, mullite fine powder, lignin and high-alumina cement according to a certain mass ratio, stirring for 20-30 minutes, and removing iron by strong magnetism again after grinding;
(3) Pouring and blank making: mixing the powder prepared in the step (2), micro silicon powder, paper pulp and water, pouring the mixture into a mold horizontally placed on a vibration platform, and performing high-frequency vibration molding to obtain a blank body;
(4) Exhausting: after the vibration is finished, the lower vibration platform is lifted together with the die, and a handheld vibrator is used for adhering the side wall of the die to move in a Z shape to perform cross exhaust;
(5) Demolding and drying: standing the blank together with the mold for 16-24 hours, demolding, naturally curing for a period of time after demolding, and then placing into a drying chamber for drying;
(6) High-temperature calcination: putting the blank dried in the step (5) into a high-temperature kiln, heating to 100-110 ℃ within 10-12 hours, keeping the temperature for 24-40 hours, heating to 500-505 ℃ within 40-80 hours, keeping the temperature for 12-24 hours, heating to 900-910 ℃ within 72-100 hours, keeping the temperature for 24-48 hours, heating to 1200-1205 ℃ within 90-160 hours, keeping the temperature for 20-30 hours, heating to 1520-1525 ℃ within 75-95 hours, keeping the temperature for 15-18 hours, cooling to 105-110 ℃ within 36-72 hours, opening the kiln, cooling, and performing post-treatment to obtain the large-scale float glass melting kiln high-temperature sillimanite pool bottom large brick;
wherein:
after the natural sillimanite raw material is fed into a factory, defective ores are removed, the natural sillimanite raw material is crushed and then carefully selected, and is screened into three granularity grades, wherein the three granularity grades comprise 0.5-1mm, 1-3mm, 18-22 mm and 3-5mm in percentage by weight, and the defective ores, the three granularity grades are subjected to strong magnetic iron removal before being distributed into different bins;
in the step (2), the sum of the mass of the sillimanite, the synthetic mullite, the refractory clay, the fine mullite powder, the mass of the lignin and the high alumina cement is 100 percent; wherein: 50-70% of sillimanite, 10-20% of synthetic mullite, 10-15% of refractory clay, 5-10% of mullite fine powder, 3-5% of lignin and 1-5% of high alumina cement.
2. The method for preparing the large-sized high-temperature sillimanite pool bottom brick for the large-sized float glass melting furnace according to claim 1, wherein the method comprises the following steps: in the step (1), after the natural sillimanite raw material is fed into a factory, defective ores are removed, the natural sillimanite raw material is crushed, selected and screened into three granularity grades, wherein the three granularity grades comprise 0.5-1mm, 1-3mm and 3-5mm in percentage by weight, and iron is removed in a strong magnetic mode before the natural sillimanite raw material is fed into different bins.
3. The method for preparing the large-sized high-temperature sillimanite pool bottom brick for the large-sized float glass melting furnace according to claim 1, wherein the method comprises the following steps: step (2) of loading a strong forceStirring in a double-shaft stirrer for 20-30 minutes; the sillimanite comprises the following chemical components: siO 2 2 35-38%、Al 2 O 3 58-60%、Fe 2 O 3 0.5 to 1.0 percent; the refractory clay comprises the following chemical components: siO 2 2 46-51%，Al 2 O 3 39-42%，Fe 2 O 3 1.5 to 2.5 percent; the granularity of the mullite fine powder is 0.5-1.5mm; the high-alumina cement is CA50-A600; the micro silicon powder comprises the following chemical components: siO 2 2 75-95%、Al 2 O 3 0.8-1.1%、Fe 2 O 3 0.6-0.9%、MgO 0.6-0.8%、CaO 0.2-0.4%、Na 2 O1.1-1.2%, and the granularity is 200 meshes.
4. The method for preparing the large-sized high-temperature sillimanite pool bottom brick for the large-sized float glass melting furnace according to claim 1, wherein the method comprises the following steps: the mass of the added silica fume in the step (3) accounts for 1-3% of the powder prepared in the step (2); the mass of the water added in the step (3) accounts for 5-10% of the powder prepared in the step (2); the mass of the added paper pulp in the step (3) accounts for 1-3% of the powder prepared in the step (2).
5. The method for preparing the large-sized high-temperature sillimanite pool bottom brick for the large-sized float glass melting furnace according to claim 1, wherein the method comprises the following steps: in the step (3), the high-frequency vibration frequency is 80-100 times/min, and the time is less than 40min; the size of the die in the step (3) is as follows: the length is 1200-5000mm, the width is 800-2000mm, and the height is 500-1000mm.
6. The method for preparing the large-sized high-temperature sillimanite pool bottom brick for the large-sized float glass melting furnace according to claim 1, wherein the method comprises the following steps: the times of cross exhaust in the step (4) are 4-6, and the exhaust process is completed within 3 minutes.
7. The method for preparing the large-sized high-temperature sillimanite pool bottom brick for the large-sized float glass melting furnace according to claim 1, wherein the method comprises the following steps: in the step (5), the natural curing temperature is 15-30 ℃, and the time is 24-48h; the drying temperature is 45-65 ℃.
8. The method for preparing the large-sized high-temperature sillimanite pool bottom brick for the large-sized float glass melting furnace according to claim 1, wherein the method comprises the following steps: and (6) in the post-treatment step, cutting the brick into proper size and shape according to the design requirement of the melting furnace, and polishing six surfaces of the large brick at the bottom of the tank to be smooth, wherein the size tolerance is controlled to be +0 mm-1 mm.
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