CN111187061A - Aluminum silicon carbide nitrogen refractory product for blast furnace tuyere and preparation method thereof - Google Patents
Aluminum silicon carbide nitrogen refractory product for blast furnace tuyere and preparation method thereof Download PDFInfo
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- CN111187061A CN111187061A CN202010096324.5A CN202010096324A CN111187061A CN 111187061 A CN111187061 A CN 111187061A CN 202010096324 A CN202010096324 A CN 202010096324A CN 111187061 A CN111187061 A CN 111187061A
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Abstract
An aluminum silicon carbide nitrogen refractory product for a blast furnace tuyere is prepared by performing co-grinding and wet grinding on plate-shaped corundum aggregate, plate-shaped corundum fine powder, silicon carbide fine powder, metal silicon powder and an additive at a temperature of over 1480 ℃ through nitriding and sintering; wherein the raw materials are added in parts by weight: 50-70 parts of tabular corundum aggregate, 2-26 parts of tabular corundum fine powder, 7-15 parts of silicon carbide fine powder and 8-30 parts of metal silicon powder; the additive accounts for 1.8 to 5 percent of the total weight of the raw materials. The aluminum silicon carbide nitrogen refractory product prepared by the invention has all the characteristics of a silicon carbide product, and the heat conductivity coefficient is only 6-8W/(m.K) at 200 ℃, and is reduced by 4-5 times compared with 30-35W/(m.K) at 200 ℃ of silicon carbide.
Description
Technical Field
The invention relates to the technical field of refractory materials, in particular to an aluminum silicon carbide nitrogen refractory product for a blast furnace tuyere and a preparation method thereof.
Background
With the increase of the large-scale blast furnace and the smelting strength, the maintenance of the furnace body is more and more emphasized, the tuyere is used as one of the key parts of the blast furnace, the service life of the blast furnace is directly influenced by the use effect, the tuyere area is subjected to severe conditions of high temperature, large load resistance and the like in the production of the blast furnace, and the tuyere bears the corrosion of high temperature, rapid change of temperature difference, alkali-containing atmosphere in the furnace and higher load action.
Along with the upgrade and modification of blast furnace tuyere and the difference of design philosophy, the selection of materials is more and more scientific, the selected other materials have shorter service life and more serious loss, and the selected silicon carbide product often can generate higher heat conductivity coefficient, so that the heat loss is more serious and the energy consumption is high.
Disclosure of Invention
The aluminum silicon carbide nitrogen refractory product prepared by the invention has all the characteristics of a silicon carbide product, and the heat conductivity coefficient of the aluminum silicon carbide nitrogen refractory product at 200 ℃ is only 6-8W/(m.K), and is reduced by 4-5 times compared with 30-35W/(m.K) at 200 ℃ of silicon carbide.
The technical scheme adopted by the invention for realizing the purpose is as follows: an aluminum silicon carbide nitrogen refractory product for a blast furnace tuyere is prepared by performing co-grinding and wet grinding on plate-shaped corundum aggregate, plate-shaped corundum fine powder, silicon carbide fine powder, metal silicon powder and an additive at a temperature of over 1480 ℃ through nitriding and sintering; wherein the raw materials are added in parts by weight: 50-70 parts of tabular corundum aggregate, 2-26 parts of tabular corundum fine powder, 7-15 parts of silicon carbide fine powder and 8-30 parts of metal silicon powder; the additive accounts for 1.8 to 5 percent of the total weight of the raw materials.
In the invention, because the silicon carbide with excellent thermal conductivity and the corundum with low thermal conductivity are adopted to replace the prior high-thermal-conductivity blast furnace tuyere refractory product, the problems of more serious heat loss and high energy consumption of the currently used materials are solved.
In the invention, the raw material has the following index requirements: plate-like corundum Al2O3≥99%，Fe2O3Not more than 0.2 percent, silicon metal powder Si not less than 98.5 percent, α -Al2O3≥98%。
Wherein, the particle size distribution of the plate-shaped corundum aggregate is 3-1mm, 1-0.5mm and 0.5-0.2mm, and the three types of particles are reasonably matched, so that the closest packing can be achieved, and the compactness of the product is improved.
Wherein the particle size distribution of the plate-shaped fine powder is 0-0.045 mm.
The additive is a plurality of compounds of sodium tripolyphosphate, paper pulp, dextrin and water.
A preparation method of an aluminum silicon carbide nitrogen refractory product for a blast furnace tuyere comprises the following steps: taking the raw materials and the additive according to the weight parts, then premixing plate-shaped corundum fine powder, silicon carbide fine powder and metal silicon powder, and co-grinding for 25-30min in a ball mill to form co-ground powder for later use; step two, mixing the tabular corundum aggregate for 1-2min, then adding a proper amount of water, mixing for 2-3min, then adding an additive, mixing for 2-3min, adding the milled powder prepared in the step one, performing net mixing for 25-30min, and then performing grinding and sieving to form pug; and step three, pressing and molding the pug, drying, and then nitriding and sintering at the temperature of at least 1480 ℃ for more than 14 hours to obtain the aluminum silicon carbide nitrogen refractory product.
Corundum has low heat conduction, silicon carbide has high heat conduction, and the single corundum or silicon carbide material is difficult to meet the requirements of low heat conduction and good alkali resistance, and the nitriding firing is a violent exothermic reaction at high temperature, and the silicon carbide has high heat conduction, so that the silicon flowing phenomenon caused by local overheating is avoided, and the quality of the product and the uniformity of components are improved.
Wherein, the drying process comprises the following steps: electrifying to-30 ℃, preserving heat for 3h at 30 ℃, then heating to 30-50 ℃, preserving heat for 10-15h at 50 ℃, then heating to 50-80 ℃, preserving heat for 6-20h at 80 ℃, heating to 80-110 ℃, preserving heat for 8-15h at 110 ℃, heating to 110-150 ℃, preserving heat for 6-10h at 150 ℃, heating to 150 ℃, and then stopping power supply and cooling.
Wherein, the nitriding and sintering process comprises the following steps: the dried product enters a kiln for secondary damp elimination, the kiln is preheated to 500 ℃, then the vacuum pumping is carried out, high-purity nitrogen is introduced, the temperature in the kiln is burnt to 1140 ℃, the heat preservation is carried out for 2 to 10 hours at 1140 ℃, then the product is burnt for 58 to 80 hours at 1140-plus 1420 ℃, the heat preservation is carried out for 8 to 14 hours at 1420 ℃, then the product is burnt for 20 hours at 1420-plus 1480 ℃, the heat preservation is carried out for 14 to 20 hours at 1480 ℃, then the product is burnt for 20 hours at 1480-plus 1500 ℃, the heat preservation is carried out for 8 to 12 hours at 1500 ℃, the nitrogen flow at 1140-plus 1500 ℃ is 13m3/h。
α -Al is present in the plate corundum2O3、γ-Al2O3Crystalline phase, it has been found that the formulation of the present invention generates Si during sintering3N4And trace amounts of Sialon phase, resulting in Si3N4Can enter the pores of the product, thereby improving the density of the product; part of crystalline phase in corundum is reduced and nitrided at high temperature and then made of AlN and Si3N4、α-Al2O3The Sialon (Sialon) is formed in a small amount by solid solution, has high bonding strength, and can improve the physical properties of the material.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
the silicon carbide selected by the invention has good heat-conducting property, the corundum has lower heat-conducting coefficient, the proportion relation of the silicon carbide and the corundum is comprehensively utilized, the heat-conducting coefficient of the prepared product is only 6-8W/(m.K) at 200 ℃, and the condition of heat loss caused by high heat conduction does not occur.
The invention is nitrided and sintered to make the metal silicon powder and nitrogen react to generate Si3N4Avoiding the direct addition of Si3N4The sintering performance of the product is not good due to the raw materials.
By adopting the specific proportion and the process measures, the prepared aluminum silicon carbide nitrogen refractory product perfectly solves the problems of high heat conduction, poor physical properties, poor alkali resistance and the like of the current material.
The technical indexes of the invention are as follows: the heat conductivity coefficient is only 6-8W/(m.K) at 200 ℃, and the original compressive strength is more than or equal to 170 MPa; the rear compressive strength is more than or equal to 160 MPa; the strength change rate is less than or equal to 6.7 percent; the volume change rate is less than or equal to 5.8 percent.
Detailed Description
The technical result is only to express the embodiment of the invention, the description is more specific and detailed, but not to be understood as the limitation of the patent scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Example 1
Preparing co-milled powder:
proportioning: 0-0.045mm of ten thousand-side plate-shaped corundum: 175 portions of
Silicon carbide fine powder: 128 parts of
Metallic silicon powder (180 mesh): 89 portions of
Sodium tripolyphosphate: 1.5 parts of
Co-milling time: and (5) 25-30 min.
At least 4 magnets are suspended below the ball mill, and scrap iron on the magnets is cleaned every time when one grinding material is discharged.
And cleaning the site and related equipment before operation.
Proportioning mud materials: 65 parts of tabular corundum aggregate, 35 parts of co-ground powder, 8 parts of dextrin powder, 5 parts of pulp powder and 9-11 parts of water. Wherein the weight ratio of the tabular corundum aggregate of 3-1mm, 1-0.5mm and 0.5-0.2mm is 7: 3: 2.
adding plate-shaped corundum 3-1mm, 1-0.5mm and 0.5-0.2mm, mixing for 1-2min, adding water, mixing for 2-3min, and adding paper pulp and dextrin; adding the milled powder after mixing for 2-3 minutes, and performing grinding and sieving after net mixing for 25-30 minutes, wherein the pug is required to be uniform and has no pug. 3 magnets must be hung below the wet mill, and scrap iron on the magnets must be cleaned every next grinding.
Granularity and moisture of pug:
the drying curve is as follows:
electrifying to-30 ℃, preserving heat for 3h at 30 ℃, then heating to 30-50 ℃, preserving heat for 10h at 50 ℃, then heating to 50-80 ℃, preserving heat for 6h at 80 ℃, heating to 80-110 ℃, preserving heat for 12h at 110 ℃, heating to 110-150 ℃, preserving heat for 6h at 150 ℃, and stopping power and cooling after heating to 150-155 ℃. The dried blank can be loaded on a truck with the residual moisture less than or equal to 2.5 percent, and the blank with the residual moisture more than 2.5 percent needs to be returned to the dryer for re-drying until the residual moisture is qualified.
The in-kiln firing curve is as follows:
the nitriding and sintering process comprises the following steps: putting the dried product into a kiln for secondary damp-retention, preheating the inside of the kiln to 500 ℃, vacuumizing and introducing high-purity nitrogen, putting the dried product into the kiln, firing the dried product to 1140 ℃, preserving heat for 10h at 1140 ℃, firing the dried product for 58h at 1140-3The allowable fluctuation range of the flow of the nitrogen is 0 to +3m3/h。
Example 2
Preparing co-milled powder:
proportioning: 0-0.045mm of ten thousand-side plate-shaped corundum: 25 portions of
Silicon carbide fine powder: 79 portions of
Metallic silicon powder (180 mesh): 288.5 parts
Sodium tripolyphosphate: 1.5 parts of
Co-milling time: and (5) 25-30 min.
At least 4 magnets are suspended below the ball mill, and scrap iron on the magnets is cleaned every time when one grinding material is discharged.
And cleaning the site and related equipment before operation.
Proportioning mud materials: 50 parts of tabular corundum aggregate, 50 parts of co-ground powder, 9 parts of dextrin powder, 11 parts of pulp powder and 10 parts of water. Wherein the plate-shaped corundum aggregate with the weight ratio of 3-1mm, 1-0.5mm and 0.5-0.2mm is 8: 3: 1.
adding plate-shaped corundum 3-1mm, 1-0.5mm and 0.5-0.2mm, mixing for 1-2min, adding water, mixing for 2-3min, and adding paper pulp and dextrin; adding the milled powder after mixing for 2-3 minutes, and performing grinding and sieving after net mixing for 25-30 minutes, wherein the pug is required to be uniform and has no pug. 3 magnets must be hung below the wet mill, and scrap iron on the magnets must be cleaned every next grinding.
The drying curve is as follows:
electrifying to-30 ℃, preserving heat for 3h at 30 ℃, then heating to 30-50 ℃, preserving heat for 15h at 50 ℃, then heating to 50-80 ℃, preserving heat for 20h at 80 ℃, heating to 80-110 ℃, preserving heat for 15h at 110 ℃, heating to 110-150 ℃, preserving heat for 8h at 150 ℃, and stopping power and cooling after heating to 150-155 ℃. The dried blank can be loaded on a truck with the residual moisture less than or equal to 2.5 percent, and the blank with the residual moisture more than 2.5 percent needs to be returned to the dryer for re-drying until the residual moisture is qualified.
The in-kiln firing curve is as follows:
the nitriding and sintering process comprises the following steps: putting the dried product into a kiln for secondary damp-retention, preheating the inside of the kiln to 500 ℃, vacuumizing and introducing high-purity nitrogen, putting the dried product into the kiln, firing the dried product to 1140 ℃, preserving heat for 8h at 1140 ℃, firing the dried product for 78h at 1140 and 1420 ℃, preserving heat for 8h at 1420 ℃, firing the dried product for 20h at 1420 and 1480 ℃, preserving heat for 20h at 1480 ℃, firing the dried product for 20h at 1480 and 1500 ℃, preserving heat for 10h at 1500 ℃, and keeping the nitrogen flow at 1140 and 1500 ℃ to 13m3The allowable fluctuation range of the flow of the nitrogen is 0 to +3m3/h。
Example 3
Preparing co-milled powder:
proportioning: 0-0.045mm of plate-shaped corundum: 132 portions of
Silicon carbide fine powder: 114 portions of
Metallic silicon powder (180 mesh): 146 portions of
Sodium tripolyphosphate: 1.5 parts of
Co-milling time: and (5) 25-30 min.
At least 4 magnets are suspended below the ball mill, and scrap iron on the magnets is cleaned every time when one grinding material is discharged.
And cleaning the site and related equipment before operation.
Proportioning mud materials: 70 parts of tabular corundum aggregate, 30 parts of co-ground powder, 8 parts of dextrin powder, 10 parts of pulp powder and 11 parts of water. Wherein the plate-shaped corundum aggregate with the weight ratio of 3-1mm, 1-0.5mm and 0.5-0.2mm is 8: 2: 2.
adding plate-shaped corundum 3-1mm, 1-0.5mm and 0.5-0.2mm, mixing for 1-2min, adding water, mixing for 2-3min, and adding paper pulp and dextrin; adding the milled powder after mixing for 2-3 minutes, and performing grinding and sieving after net mixing for 25-30 minutes, wherein the pug is required to be uniform and has no pug. 3 magnets must be hung below the wet mill, and scrap iron on the magnets must be cleaned every next grinding.
The drying curve is as follows:
electrifying to-30 ℃, preserving heat for 3h at 30 ℃, then heating to 30-50 ℃, preserving heat for 14h at 50 ℃, then heating to 50-80 ℃, preserving heat for 18h at 80 ℃, heating to 80-110 ℃, preserving heat for 8h at 110 ℃, heating to 110-150 ℃, preserving heat for 10h at 150 ℃, and stopping power and cooling after heating to 150-155 ℃. The dried blank can be loaded on a truck with the residual moisture less than or equal to 2.5 percent, and the blank with the residual moisture more than 2.5 percent needs to be returned to the dryer for re-drying until the residual moisture is qualified.
The in-kiln firing curve is as follows:
the nitriding and sintering process comprises the following steps: putting the dried product into a kiln for secondary damp-retention, preheating the inside of the kiln to 500 ℃, vacuumizing and introducing high-purity nitrogen, putting the dried product into the kiln, burning the inside of the kiln to 1140 ℃, preserving heat for 2h at 1140 ℃, then burning the dried product for 60h at 1140 and 1420 ℃, preserving heat for 14h at 1420 ℃, then burning the dried product for 20h at 1420 and 1480 ℃, preserving heat for 14h at 1480 ℃, then burning the dried product for 20h at 1480 and 1500 ℃ and preserving heat for 12h at 1500 ℃, wherein the nitrogen flow at 1140 and 1500 ℃ is 13m3The allowable fluctuation range of the flow of the nitrogen is 0 to +3m3/h。
Example 4
Preparing co-milled powder:
proportioning: 0-0.045mm of plate-shaped corundum: 256.5 portions
Silicon carbide fine powder: 105 portions of
Metallic silicon powder (180 mesh): 132 portions of
Sodium tripolyphosphate: 1.5 parts of
Co-milling time: and (5) 25-30 min.
Proportioning mud materials: 60 parts of tabular corundum aggregate, 40 parts of co-ground powder, 7 parts of dextrin powder, 12 parts of pulp powder and 12 parts of water. Wherein the weight ratio of the tabular corundum aggregate of 3-1mm, 1-0.5mm and 0.5-0.2mm is 35: 16: 10. the preparation process is as in example 1.
The results of the physicochemical analyses of the articles obtained in examples 1 to 4 are given in the following table:
Claims (7)
1. the utility model provides an aluminium carborundum nitrogen refractory product for blast furnace tuyere which characterized in that: the raw materials are plate corundum aggregate, plate corundum fine powder, silicon carbide fine powder, metal silicon powder and admixture, and the mixture is formed by co-grinding, wet grinding and nitriding firing at the temperature of over 1480 ℃; wherein the raw materials are added in parts by weight: 50-70 parts of tabular corundum aggregate, 2-26 parts of tabular corundum fine powder, 7-15 parts of silicon carbide fine powder and 8-30 parts of metal silicon powder; the additive accounts for 1.8 to 5 percent of the total weight of the raw materials.
2. The aluminum silicon carbide nitrogen refractory for a tuyere of a blast furnace as set forth in claim 1, wherein: the particle size distribution of the plate-shaped corundum aggregate is 3-1mm, 1-0.5mm and 0.5-0.2 mm.
3. The aluminum silicon carbide nitrogen refractory for a tuyere of a blast furnace as set forth in claim 1, wherein: the particle size distribution of the plate-shaped fine powder is 0-0.045 mm.
4. The aluminum silicon carbide nitrogen refractory for a tuyere of a blast furnace as set forth in claim 1, wherein: the additive is a plurality of compounds of sodium tripolyphosphate, paper pulp, dextrin and water.
5. The method for preparing the aluminum silicon carbide nitrogen refractory product for the tuyere of the blast furnace as claimed in claim 1, comprising the steps of:
taking the raw materials and the additive according to the weight parts, then premixing plate-shaped corundum fine powder, silicon carbide fine powder and metal silicon powder, and co-grinding for 25-30min in a ball mill to form co-ground powder for later use;
step two, mixing the tabular corundum aggregate for 1-2min, then adding a proper amount of water, mixing for 2-3min, then adding an additive, mixing for 2-3min, adding the milled powder prepared in the step one, performing net mixing for 25-30min, and then performing grinding and sieving to form pug;
and step three, pressing and molding the pug, drying, and then nitriding and sintering at the temperature of at least 1480 ℃ for more than 14 hours to obtain the aluminum silicon carbide nitrogen refractory product.
6. The method for preparing an aluminum silicon carbide nitrogen refractory product for a blast furnace tuyere according to claim 5, wherein the drying process comprises: electrifying to-30 ℃, preserving heat for 3h at 30 ℃, then heating to 30-50 ℃, preserving heat for 10-15h at 50 ℃, then heating to 50-80 ℃, preserving heat for 6-20h at 80 ℃, heating to 80-110 ℃, preserving heat for 8-15h at 110 ℃, heating to 110-150 ℃, preserving heat for 6-10h at 150 ℃, heating to 150 ℃, and then stopping power supply and cooling.
7. The method for preparing the aluminum silicon carbide nitrogen refractory product for the blast furnace tuyere of claim 5, wherein the nitriding firing process comprises: the dried product enters a kiln for secondary damp elimination, the kiln is preheated to 500 ℃, then the vacuum pumping is carried out, high-purity nitrogen is introduced, the temperature in the kiln is burnt to 1140 ℃, the heat preservation is carried out for 2 to 10 hours at 1140 ℃, then the product is burnt for 58 to 80 hours at 1140-plus 1420 ℃, the heat preservation is carried out for 8 to 14 hours at 1420 ℃, then the product is burnt for 20 hours at 1420-plus 1480 ℃, the heat preservation is carried out for 14 to 20 hours at 1480 ℃, then the product is burnt for 20 hours at 1480-plus 1500 ℃, the heat preservation is carried out for 8 to 12 hours at 1500 ℃, the nitrogen flow at 1140-plus 1500 ℃ is 13m3/h。
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