CN110483023B - Microporous corundum brick and preparation method thereof - Google Patents
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Abstract
The invention discloses a microporous corundum brick and a preparation method thereof. The microporous corundum brick mainly comprises 75-95% of compact corundum, 0-10% of andalusite, 0-8% of silicon carbide, 3-5% of combined clay powder and 0.4-2% of metal silicon micropowder. Dry mixing the compact corundum or the compact corundum and andalusite as aggregate; then adding phenolic resin for mixing; then adding silicon carbide, combined clay powder and metal silicon micro powder or combined clay powder and metal silicon micro powder, and mixing and grinding to obtain a mixed material; pressing the mixed material into a green brick; and drying and sintering the green brick in sequence to obtain the product of the microporous corundum brick. The refractory product prepared by the method has moderate heat-conducting property, high compressive strength, excellent erosion resistance, scouring resistance and excellent thermal shock stability, can be fired in an open oxidizing atmosphere, has high production efficiency, can meet the harsh process requirements of large-scale blast furnace ceramic cups, and has excellent use effect.
Description
The technical field is as follows:
the invention relates to a refractory material and a preparation method thereof, in particular to a microporous corundum brick and a preparation method thereof.
Secondly, background art:
realizing the long service life and large-scale of the blast furnace is an important target of the iron-making industry. With the continuous deepening and strong promotion of energy saving, consumption reduction and energy saving and emission reduction work in the ferrous metallurgy industry in China, the development of the refractory material suitable for the long service life of the blast furnace is one of the research key points in the field of new materials. The long service life of the blast furnace is a system engineering, and the refractory material for the blast furnace body plays an important role in the system engineering.
In recent years, the working condition environment of a blast furnace is more and more severe due to the adoption of economic materials and the intensified smelting in the steel industry, the corrosion of slag, the corrosion of alkali and the like are greatly enhanced, and the refractory material of the furnace hearth is required to have stronger corrosion resistance under the condition. In addition, theories and practices show that the aperture is controlled, and the use performances of the material such as slag resistance and the like can be improved by increasing the proportion of micropores. The microporous refractory material not only has longer service life than the market application product, but also plays an important energy-saving role in the use process, and is gradually accepted by more and more steel design houses and steel companies in recent years.
At present, the production and manufacture of microporous refractory materials adopt reducing atmosphere firing, and two ways are generally adopted: inert gas protection and carbon burying sintering. The firing equipment for inert gas protection is complex, and large or ultra-large size products are not easy to produce. The carbon burying and burning procedures are multiple, the industrial production efficiency is low, the dust is large in the carbon burying and brick discharging processes of the product, and the production environment is poor.
The corundum brick can increase the volume fraction of pores smaller than 1 μm to more than 50% under the carbon-embedded atmosphere, the average pore diameter is within 1 μm, but the corundum brick is sintered under the weak oxidizing atmosphere, the average pore diameter is still about 7 μm, the volume fraction of pores smaller than 1 μm is between 20% and 30%, and the corundum brick is sintered under the oxidizing atmosphere, and the pore diameter of micropores is less or none. The microporous sintering of the refractory material in a common oxidizing atmosphere is a problem to be solved urgently.
Thirdly, the invention content:
the technical problem to be solved by the invention is as follows: the microporous corundum brick and the preparation method thereof are provided by utilizing the existing tunnel kiln sintering production equipment and according to the environmental protection requirement. The invention combines the characteristics of a blast furnace and a microporous corundum brick, adopts raw materials of compact corundum, andalusite, silicon carbide, metal silicon micro powder and the like, prepares a brick blank after mixing, forming and drying, and then is fired at high temperature by a tunnel kiln to form the microporous corundum brick.
In order to solve the problems, the invention adopts the technical scheme that:
the invention provides a microporous corundum brick which comprises, by weight, 75-95% of compact corundum, 0-10% of andalusite, 0-8% of silicon carbide, 3-5% of combined clay powder and 0.4-2% of metal silicon micropowder.
According to the microporous corundum brick, the 75-95% of compact corundum is composed of 5-10% of compact corundum with the particle size of 5-3mm, 30-50% of compact corundum with the particle size of 3-1mm and 40-55% of compact corundum with the particle size of less than 1mm in percentage by weight.
According to the microporous corundum brick, the volume density of the dense corundum is 3.8-3.9 g/cm3。
According to the microporous corundum brick, the granularity of the silicon carbide is less than 180 meshes, and the purity of the silicon carbide is more than or equal to 97%.
According to the microporous corundum brick, the particle size of the combined clay powder is less than 180 meshes.
According to the microporous corundum brick, the granularity of the metal silicon micro powder is less than 1 mu m, and the mass percentage content of Si in the metal silicon micro powder is more than or equal to 95%.
The granularity of the andalusite is determined according to the micropore corundum brick<1mm, Al in andalusite2O3The mass percentage content of the compound is more than or equal to 57 percent.
In addition, the preparation method of the microporous corundum brick comprises the following steps:
a. firstly, weighing various raw materials according to the proportion of the microporous corundum brick;
b. pouring the weighed raw materials of compact corundum or compact corundum and andalusite as aggregate into a mixer for dry mixing for 1-2 minutes; then adding phenolic resin accounting for 2-3% of the total weight of all the raw materials, and mixing for 3-5 minutes; then adding the weighed raw materials of silicon carbide, combined clay powder and metal silicon micro powder or combined clay powder and metal silicon micro powder, and mixing and grinding for 15-25 minutes to obtain a mixed material;
c. c, pressing and forming the mixed material obtained in the step b by using a forming press to obtain a green brick;
d. drying the green bricks subjected to compression molding in a drying kiln for 24-36 hours, wherein the temperature of a vehicle entrance of the drying kiln is less than 90 ℃, and the highest drying temperature is controlled at 110-180 ℃;
e. and d, firing the dried green bricks in the step d in an oxidizing atmosphere by adopting a high-temperature tunnel kiln or a shuttle kiln, wherein the firing temperature is 1420-1550 ℃, keeping the temperature for 4-8 h when reaching the firing temperature, and cooling to room temperature after keeping the temperature to obtain the microporous corundum bricks.
According to the preparation method of the microporous corundum brick, the forming pressure of the forming press in the step c is 400-1000 tons; the volume density of the obtained green brick is 3.10-3.35 g/cm3。
According to the preparation method of the microporous corundum brick, the specific heating process of the sintering in the step e is as follows: heating the temperature from normal temperature to 450 ℃ for 10-14 h; raising the temperature from 450 ℃ to 850 ℃ after 12-16 h; raising the temperature from 850 ℃ to 1250-1300 ℃ after 16-24 hours; raising the temperature from 1250-1300 ℃ to 1500-1550 ℃ after 20-26 h; preserving the heat for 4-8 h at 1500-1550 ℃; and then reducing the temperature from 1500-1550 ℃ to 800 ℃ for 12-16 h, and finally reducing the temperature from 800 ℃ to room temperature for 10-14 h, and taking the product out of the kiln.
The invention has the following positive beneficial effects:
1. the refractory product prepared by the technical scheme of the invention has moderate heat-conducting property, high compressive strength, excellent erosion resistance, scouring resistance and excellent thermal shock stability, can be fired in an open oxidizing atmosphere, has high production efficiency, can meet the harsh technological requirements of large-scale blast furnace ceramic cups, and has excellent use effect.
2. In the process of sintering the microporous corundum brick, the metal silicon micro powder in the technical scheme is gradually oxidized from 200 ℃ to about 450 ℃ to form an oxide film, so that oxygen is prevented from permeating into the brick body, and carbon in silicon carbide and phenolic resin is effectively protected from being oxidized.
3. The granularity of the metallic silicon micro powder in the technical scheme of the invention<1 μm, forms a micropore in the oxidation process, and the density of the obtained product micropore corundum brick is 3.10g/cm3The porosity is less than 12%, wherein the aperture is less than 1 μm and accounts for more than 60%, and the slag erosion resistant depth is less than 2 mm; the density of the common ceramic cup material is 3.05g/cm3About, the depth of slag erosion resistance is more than 14 mm.
Fourthly, the specific implementation mode:
the invention is further illustrated by the following examples, which do not limit the scope of the invention.
In the following examples: the volume density of the adopted compact corundum is 3.8-3.9 g/cm3(ii) a Particle size of silicon carbide<180 meshes, and the purity of the silicon carbide is more than or equal to 97 percent; particle size of the bound clay<180 meshes; particle size of metallic silicon powder<1 micron, and the mass percentage of Si in the metal silicon micro powder is more than or equal to 95 percent; andalusite particle size<1mm, Al in andalusite2O3The mass percentage content of the compound is more than or equal to 57 percent. In addition, the dense corundum includes 5-3mm dense corundum, 3-1mm dense corundum and<1mm of dense corundum, wherein<1mm dense corundum is divided into 1-0mm dense corundum and 180-mesh dense corundum; andalusite particle size<1mm, including 1-0mm andalusite and 180 mesh andalusite.
Example 1:
the invention relates to a microporous corundum brick, which comprises the following raw materials in percentage by weight: 5% of compact corundum with the particle size of 5-3mm, 42% of compact corundum with the particle size of 3-1mm, 18% of compact corundum with the particle size of 1-0mm, 22% of compact corundum with the particle size of 180 meshes, 8% of silicon carbide powder, 3% of bonded clay powder and 2% of metal silicon micro powder.
Example 2:
the invention relates to a microporous corundum brick, which comprises the following raw materials in percentage by weight: 10 percent of compact corundum with the grain diameter of 5-3mm, 37 percent of compact corundum with the grain diameter of 3-1mm, 13 percent of compact corundum with the grain diameter of 1-0mm, 29 percent of compact corundum with the grain diameter of 180 meshes, 5 percent of andalusite with the grain diameter of 1-0mm, 0.5 percent of silicon carbide powder, 5 percent of combined clay powder and 0.5 percent of metal silicon micro powder.
Example 3:
the invention relates to a microporous corundum brick, which comprises the following raw materials in percentage by weight: 8 percent of compact corundum with the grain diameter of 5-3mm, 30 percent of compact corundum with the grain diameter of 3-1mm, 17 percent of compact corundum with the grain diameter of 1-0mm, 23 percent of compact corundum with the grain diameter of 180 meshes, 5 percent of andalusite with the grain diameter of 1-0mm, 5 percent of andalusite with the grain diameter of 180 meshes, 6 percent of silicon carbide powder, 5 percent of combined clay powder and 1 percent of metal silicon micro powder.
The embodiment 1-3 of the invention relates to a preparation method of a microporous corundum brick, which comprises the following detailed steps:
a. firstly, weighing various raw materials according to the proportion of the microporous corundum brick in any one of embodiments 1-3;
b. pouring the weighed raw materials of compact corundum or compact corundum and andalusite as aggregate into a mixer for dry mixing for 2 minutes; then adding phenolic resin accounting for 3 percent of the total weight of all the raw materials, and mixing for 5 minutes; then adding the weighed raw materials of silicon carbide powder, bonding clay powder and metal silicon micro powder, and mixing and grinding for 20 minutes to obtain a mixed material;
c. c, pressing and molding the mixed material obtained in the step b by using a molding press, wherein the pressure of the molding press is 1000 tons, and the green brick is obtained by pressing, and the volume density of the green brick is 3.10-3.35 g/cm3；
d. Drying the green bricks subjected to compression molding in a drying kiln for 32 hours, wherein the temperature of a vehicle entrance of the drying kiln is less than 90 ℃, and the highest drying temperature is controlled to be 120-160 ℃;
e. d, firing the dried green bricks in the step d in an oxidizing atmosphere by adopting a high-temperature tunnel kiln or a shuttle kiln, keeping the temperature for 6 hours when the firing temperature is 1550 ℃, and cooling to room temperature after keeping the temperature to obtain the microporous corundum bricks;
the specific heating process of the firing is as follows: the temperature is increased from normal temperature to 450 ℃ after 12 hours; increasing the temperature from 450 ℃ to 850 ℃ after 15 h; increasing the temperature from 850 ℃ to 1300 ℃ after 20 hours; increasing the temperature from 1300 ℃ to 1550 ℃ after 22 hours; keeping the temperature at 1550 ℃ for 6 h; then the temperature is reduced from 1550 ℃ to 800 ℃ after 16h, and finally the product is taken out of the kiln after 12h and is reduced from 800 ℃ to room temperature.
The data of the performance test of the micro-porous corundum bricks prepared by the method of the invention in the examples 1-3 are shown in the table 1.
TABLE 1 data on the measurements of the relevant Properties of the products obtained in examples 1 to 3 of the present invention
Claims (2)
1. The preparation method of the microporous corundum brick is characterized by comprising the following steps:
a. the microporous corundum brick comprises 75-95% of compact corundum, 0-10% of andalusite, 0-8% of silicon carbide, 3-5% of combined clay powder and 0.4-2% of metal silicon micropowder;
the 75-95% of compact corundum is composed of 5-10% of compact corundum with the particle size of 5-3mm, 30-50% of compact corundum with the particle size of 3-1mm and 40-55% of compact corundum with the particle size of less than 1mm in percentage by weight;
the volume density of the compact corundum is 3.8-3.9 g/cm3(ii) a The grain size of the silicon carbide<180 meshes, and the purity of the silicon carbide is more than or equal to 97 percent; the granularity of the metal silicon micro powder<1 mu m, wherein the mass percentage content of Si in the metal silicon micro powder is more than or equal to 95%; particle size of the bound clay powder<180 meshes; the particle size of the andalusite<1mm, Al in andalusite2O3The mass percentage content of the compound is more than or equal to 57 percent;
b. firstly, weighing various raw materials according to the proportion of the microporous corundum brick in the step a;
c. pouring the weighed raw materials of compact corundum or compact corundum and andalusite as aggregate into a mixer for dry mixing for 1-2 minutes; then adding phenolic resin accounting for 2-3% of the total weight of all the raw materials, and mixing for 3-5 minutes; then adding the weighed raw materials of silicon carbide, combined clay powder and metal silicon micro powder or combined clay powder and metal silicon micro powder, and mixing and grinding for 15-25 minutes to obtain a mixed material;
d. c, pressing and forming the mixed material obtained in the step c by using a forming press to obtain a green brick;
e. drying the green bricks subjected to compression molding in a drying kiln for 24-36 hours, wherein the vehicle entrance temperature of the drying kiln is less than 90 ℃, and the highest drying temperature is controlled at 110-180 ℃;
f. firing the dried green bricks in the step e in an oxidizing atmosphere by adopting a high-temperature tunnel kiln or a shuttle kiln, wherein the firing temperature is 1420-1550 ℃, keeping the temperature for 4-8 h when reaching the firing temperature, and cooling to room temperature after keeping the temperature to obtain the microporous corundum bricks;
the specific heating process of the sintering is as follows: after 10-14 h, the temperature is raised to 450 ℃ from the normal temperature; raising the temperature from 450 ℃ to 850 ℃ after 12-16 h; after 16-24 h, raising the temperature from 850 ℃ to 1250-1300 ℃; raising the temperature from 1250-1300 ℃ to 1500-1550 ℃ after 20-26 h; preserving heat for 4-8 h at 1500-1550 ℃; and then reducing the temperature from 1500-1550 ℃ to 800 ℃ for 12-16 h, and finally reducing the temperature from 800 ℃ to room temperature for 10-14 h, and taking the product out of the kiln.
2. The method for preparing a microporous corundum brick according to claim 1, characterized in that: the forming pressure of the forming press in the step d is 400-1000 tons; the volume density of the obtained green brick is 3.10-3.35 g/cm3。
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| CN112645697A (en) * | 2020-12-07 | 2021-04-13 | 北京金隅通达耐火技术有限公司 | High-density corundum mullite brick for hazardous waste disposal rotary kiln |
| CN115819075A (en) * | 2022-12-10 | 2023-03-21 | 巩义通达中原耐火技术有限公司 | Low-temperature sintered titanium-rich corundum composite silicon carbide brick and preparation method thereof |
| CN116462493A (en) * | 2023-03-31 | 2023-07-21 | 巩义通达中原耐火技术有限公司 | Titanium-rich corundum composite silicon carbide unburned brick and preparation method thereof |
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| CN103467119A (en) * | 2013-08-29 | 2013-12-25 | 浙江长兴强立耐火材料有限公司 | Preparation method for microporous alumina carbon brick |
| CN103936443A (en) * | 2014-04-03 | 2014-07-23 | 巩义市第五耐火材料总厂 | Novel micropore corundum brick and preparation method thereof |
| CN109761611A (en) * | 2019-02-16 | 2019-05-17 | 通达耐火技术股份有限公司 | A kind of fiber reinforced micro porous silicon nitride compound carbonizing silica brick and preparation method thereof |
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| JP3617765B2 (en) * | 1998-01-19 | 2005-02-09 | 東芝セラミックス株式会社 | Slide gate plate and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1108634A (en) * | 1994-08-25 | 1995-09-20 | 武汉钢铁(集团)公司 | Fired microporous carbon-aluminium brick |
| CN103467119A (en) * | 2013-08-29 | 2013-12-25 | 浙江长兴强立耐火材料有限公司 | Preparation method for microporous alumina carbon brick |
| CN103936443A (en) * | 2014-04-03 | 2014-07-23 | 巩义市第五耐火材料总厂 | Novel micropore corundum brick and preparation method thereof |
| CN109761611A (en) * | 2019-02-16 | 2019-05-17 | 通达耐火技术股份有限公司 | A kind of fiber reinforced micro porous silicon nitride compound carbonizing silica brick and preparation method thereof |
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