CN112573932B - Homogeneous body re-sintered fused zirconia mullite brick and preparation method thereof - Google Patents
Homogeneous body re-sintered fused zirconia mullite brick and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of refractory materials, in particular to a homogeneous body re-sintered fused zirconia mullite brick and a preparation method thereof. The homogeneous body is sintered to obtain the fused zirconia-mullite brick, the aggregate and the matrix are zirconium-mullite mineral phases, and the fused zirconia-mullite brick is prepared from the following powder materials, cellulose dry powder and magnesium lignosulfonate stock solution in percentage by weight: 35-50% of fused zirconia mullite with the grain diameter being more than 1mm and less than or equal to 3mm, 20-30% of fused zirconia mullite with the grain diameter being more than or equal to 0.1mm and less than or equal to 1mm, 0-35% of fused zirconia mullite with the grain diameter being less than or equal to 0.045mm, 0-20% of fused white corundum with the grain diameter being less than or equal to 0.045mm, 0-10% of 65 zircon powder with the grain diameter being less than or equal to 0.045mm and 0-5% of Suzhou soil with the grain diameter being less than or equal to 0.045 mm. The homogeneous body re-sintered electric smelting zirconium mullite brick has good steam erosion resistance and thermal shock resistance of a glass kiln; the invention also provides a simple and feasible preparation method.
Description
Technical Field
The invention relates to the technical field of refractory materials, in particular to a homogeneous body re-sintered fused zirconia mullite brick and a preparation method thereof.
Background
The glass kiln is the most important thermal equipment in the glass industry. With the development of the glass industry, the temperature of the kiln is gradually increased, and the requirements on refractory materials for the kiln are continuously increased. The flame space and the feed inlet of the glass kiln are greatly influenced by atmosphere, the heat exchange is more, and the heat exchange of a passage burning gun and a top burning gun of the kiln in the top burning technology is in the condition of heat exchange, so that the refractory material is required to have good erosion resistance and thermal shock resistance.
The common zirconia-mullite brick is manufactured by using sintered or electric-fused mullite aggregate, sintered or electric-fused white corundum aggregate, zircon sand or powder, alumina powder and Suzhou soil as raw materials, wherein the erosion resistance of the electric-fused aggregate or fine powder is generally better than that of the sintered aggregate or fine powder; the mineral composition of the aggregate is mullite or corundum, and the mineral composition of the matrix is zircon mullite; the aggregate does not contain zirconia, so that the erosion resistance of the aggregate is lower than that of the matrix, and the overall erosion resistance of the product cannot achieve the optimal effect.
Patent CN103496992a discloses a chromium zirconium mullite refractory material and a preparation method thereof, wherein the preparation method comprises the following steps: the method is characterized in that fused mullite or sintered mullite is used as an aggregate, zircon powder, corundum powder and chromium oxide green are used as product matrixes, 65% of mullite, 10% of corundum powder, 15% of zircon powder and 10% of chromium oxide green are uniformly mixed in a stirrer according to the formula, about 3% of pulp liquid is added as a binder, ageing is carried out for 8 hours after uniform stirring, the mixture is directly formed by a press machine, and the mixture is dried and then is subjected to heat preservation at a high temperature of about 1650 ℃ for 4 hours to be sintered. Compared with the fused mullite brick, the alkali corrosion resistance is improved, but the introduction of chromium oxide green easily affects the environment.
Patent CN109336575A discloses a zirconium-containing re-sintered fused mullite brick and a preparation method thereof, wherein fused mullite is used as an aggregate, zircon powder, corundum powder, fused quartz powder, high-temperature alumina micro powder and the like are used as product substrates, 70% of mullite, 10% of corundum powder, 8% of zircon powder, 2% of fused quartz powder and 10% of high-temperature alumina are uniformly mixed in a stirrer according to the formula, about 3% of pulp liquid is added as a binder, ageing is carried out for 4 hours after uniform stirring, molding is directly carried out by a press, and sintering is carried out at a high temperature of about 1700 ℃ for 8 hours after drying. Compared with the fused mullite brick, the alkali corrosion resistance is improved, but a large amount of low-temperature glass phase is generated under the action of boron oxide corrosive gas in the using process, so that the burning gun brick is softened and deformed.
Disclosure of Invention
The invention aims to provide a homogeneous body re-sintered fused zirconia mullite brick which has good steam erosion resistance and thermal shock resistance of a glass kiln and is suitable for a high-temperature area of a glass melting kiln, a total oxygen combustion burning brick and a glass kiln passage burning brick; the invention also provides a simple, feasible, energy-saving and environment-friendly preparation method.
The homogeneous body resintering electrofused zirconium mullite brick is prepared by the following powder materials, cellulose dry powder and magnesium lignosulfonate stock solution in percentage by weight:
the content of the cellulose dry powder is 0.1-0.3% of the total weight of the powder;
the content of the magnesium lignosulfonate stock solution is 2-5% of the total weight of the powder.
Preferably, the homogeneous body re-sintered fused zirconia-mullite brick is prepared from the following powder materials in percentage by weight, cellulose dry powder and magnesium lignosulfonate stock solution:
the content of the cellulose dry powder is 0.1-0.3% of the total weight of the powder;
the content of the magnesium lignosulphonate stock solution is 3-5% of the total weight of the powder.
The physical and chemical indexes of the fused zirconia mullite are as follows: zrO (ZrO) 2 ：30-35％，Al 2 O 3 ：42-49％，SiO 2 ：16-20％，Fe 2 O 3 Not less than 0.3 percent and the volume density not less than 3.5g/cm 3 The apparent porosity is less than or equal to 5 percent, the mullite phase is more than or equal to 50 percent, the baddeleyite phase is more than or equal to 28 percent, the corundum phase is less than or equal to 5 percent, and the glass phase is less than or equal to 5 percent.
The fused zirconia mullite has the characteristics of uniform mineral composition, small expansion coefficient, good thermal shock resistance and good erosion resistance, and the fused zirconia mullite brick is prepared by using the fused zirconia mullite raw material and then sintered, so that the alkali vapor erosion resistance is greatly superior to that of the common zirconia mullite brick, and the thermal shock resistance is excellent.
Electric melting of white corundumThe physical and chemical indexes are as follows: al (aluminum) 2 O 3 ≥99.5％，Fe 2 O 3 ≤0.1％，Na 2 O≤0.35％。
The physicochemical indexes of 65 zircon powder are as follows: zrO (zirconium oxide) 2 ≥65％，Fe 2 O 3 ≤0.1％；Al 2 O 3 ≤0.4％。
The physicochemical indexes of Suzhou soil are as follows: al (Al) 2 O 3 ≥36％，Fe 2 O 3 Less than or equal to 0.4 percent, less than or equal to 2 percent of impurity content and less than or equal to 15 percent of ignition loss.
Wherein, the grain sizes of the electric melting white corundum, the 65 zircon powder and the Suzhou soil are required to be as follows: the weight content of the particle size of more than 0.045mm is less than or equal to 3 percent.
The preparation method of the homogeneous body resintering electrofused zirconium mullite brick comprises the following steps:
(1) Putting fused zirconia mullite with the grain size of more than 1mm and less than or equal to 3mm and the grain size of more than 0.1mm and less than or equal to 1mm into a mixer, mixing and grinding for 5-10min to ensure that coarse and fine grains are uniformly distributed, adding a magnesium lignosulfonate stock solution, mixing and grinding for 5-10min, stopping grinding and stirring for 1 time in the middle, ensuring that all raw material grains are soaked by the magnesium lignosulfonate stock solution, and obtaining mixed coarse powder;
(2) Adding the powder with the particle size of less than or equal to 0.045mm and cellulose into a cone mixer, and mixing and grinding for 3-10min to obtain mixed fine powder;
(3) Adding the mixed fine powder into the mixed coarse powder, mixing and grinding for 15-20min to obtain semi-dry pug, and ageing for 4-5h;
(4) Molding the pug after ageing into green bodies by adopting a friction press or a hydraulic press, wherein the molding pressure is 1.5-3t/cm 2 The density of the formed green body is 3.1-3.3g/cm 3 Then drying and sintering to obtain homogeneous body and then sintering the electric melting zirconium mullite brick.
In the step (4), the drying temperature is 80-120 ℃, and the time is 24-48h; the sintering temperature is 1500-1600 ℃ and the time is 6-12h.
The homogeneous body is not shrunk in size in the sintering process of the electric melting zirconium mullite brick, the accuracy of the size and the shape of the product can be kept, and net size molding can be realized.
Prepared by the inventionThe physical and chemical indexes of the homogeneous body re-sintered fused zirconia mullite brick are as follows: al (Al) 2 O 3 ：47-55％，Fe 2 O 3 ≤0.2％，ZrO 2 ：27-32％，SiO 2 :15-20%, impurity content less than 0.9%, porosity less than or equal to 16%, volume density more than or equal to 3.00g/cm 3 The normal temperature compressive strength is more than or equal to 100MPa, the 0.2MPa refractoriness under load temperature T 0.6 More than or equal to 1700 ℃, the change of the dead burning line at 1650 ℃ is less than 0.1 percent, and the thermal expansion rate at 1400 ℃ is less than 0.65 percent.
Compared with the prior art, the invention has the following beneficial effects:
(1) The aggregate and the matrix of the invention both adopt the fused zirconia mullite, and the sintered zirconia mullite homogeneous body generated by the reaction has consistent thermal expansion rate, and even and consistent thermal shock resistance and erosion resistance;
(2) The invention ensures that the product achieves the optimal molding volume density by limiting the molding pressure of unit area, and simultaneously avoids the product looseness, low strength and erosion resistance caused by too small molding pressure or the elastic aftereffect caused by too large molding pressure and the cracks of the semi-finished product after molding;
(3) According to the invention, the zircon powder and the white corundum powder react at high temperature, the volume expansion and the sintering shrinkage are mutually offset, and the product is not shrunk and expanded in the sintering process, so that the accuracy of the size and the shape of the product can be kept, the net size forming is achieved, the sintering shrinkage deformation is prevented, the product qualification rate is high, and no post-processing is required;
(4) The invention mixes the substrate fine powder and cellulose uniformly in advance, which not only improves the plasticity of the pug and is beneficial to forming, but also ensures the reaction uniformity of the substrate in the sintering process;
(5) The homogeneous body re-sintered electrically fused zirconia mullite brick has good steam erosion resistance and thermal shock resistance of a glass kiln, and is suitable for a high-temperature area of a glass melting kiln, a total oxygen combustion lance brick and a glass kiln passage lance brick.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described below by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Examples 1 to 10
The homogeneous body re-sintered fused zirconia-mullite bricks of examples 1-10 were made from the materials of the following types, sizes and weight percentages as shown in table 1, wherein the total weight of the powders was 100%, and the total weight of the cellulose powder and the magnesium lignosulfonate stock solution was 100%.
Table 1 raw material type, particle size specification and weight percentages of examples 1-10
The homogeneous body re-sintered fused zirconia mullite brick is prepared according to the raw material formula in the table 1, and comprises the following steps:
(1) Putting fused zirconia mullite with the grain size of more than 1mm and less than or equal to 3mm and the grain size of more than 0.1mm and less than or equal to 1mm into a mixer, mixing and grinding for 5min to ensure that coarse and fine grains are uniformly distributed, adding a magnesium lignosulfonate stock solution, mixing and grinding for 5min, stopping grinding and stirring for 1 time in the middle, ensuring that all raw material grains are soaked by the magnesium lignosulfonate stock solution, and obtaining mixed coarse powder;
(2) Adding the powder with the particle size of less than or equal to 0.045mm and cellulose into a cone mixer, and mixing and grinding for 3min to obtain mixed fine powder;
(3) Adding the mixed fine powder into the mixed coarse powder, mixing and grinding for 15min to prepare semi-dry pug, and ageing for 4h;
(4) Molding the pug after ageing into green bodies by adopting a friction press, wherein the molding pressure is 2t/cm 2 The density of the formed green compact is 3.1-3.3g/cm 3 And then, keeping the temperature at 100 ℃ for 24h for drying, and then keeping the temperature at 1580 ℃ for 12h for sintering to obtain a homogeneous body and then sintering the fused zirconia-mullite brick.
Comparative example 1
The comparative example adopts mullite aggregate, and the types, the granularity specifications and the weight percentages of the powder are as follows:
the preparation steps are as follows:
(1) Putting mullite with the grain size of more than 1mm and less than or equal to 3mm and the grain size of more than 0.1mm and less than or equal to 1mm into a mixer, mixing and grinding for 5min to ensure that coarse and fine grains are uniformly distributed, adding magnesium lignosulfonate stock solution, mixing and grinding for 5min, stopping grinding and stirring for 1 time in the middle, ensuring that all raw material grains are soaked by the magnesium lignosulfonate stock solution, and obtaining mixed coarse powder;
(2) Adding powder with the particle size of less than or equal to 0.045mm into the mixed coarse powder, mixing and grinding for 15min to prepare semi-dry pug, and ageing for 4h;
(3) Molding the pug after ageing into green bodies by adopting a friction press, wherein the molding pressure is 2t/cm 2 The density of the formed green compact is 3.1-3.3g/cm 3 And then, keeping the temperature at 100 ℃ for 24h for drying, and then keeping the temperature at 1580 ℃ for 12h for firing to obtain the mullite brick.
Comparative example 2
The comparative example adopts the electro-fused white corundum aggregate, and the types, the granularity specifications and the weight percentages of the powder are as follows:
the preparation steps are as follows:
(1) Putting the fused white corundum with the grain size of more than 1mm and less than or equal to 3mm and the grain size of more than 0.1mm and less than or equal to 1mm into a mixer, mixing and grinding for 5min to ensure that coarse and fine grains are uniformly distributed, adding the magnesium lignosulfonate stock solution, mixing and grinding for 5min, stopping grinding and stirring for 1 time in the middle, ensuring that all raw material grains are soaked by the magnesium lignosulfonate stock solution, and obtaining mixed coarse powder;
(2) Adding powder with the particle size of less than or equal to 0.045mm into the mixed coarse powder, mixing and grinding for 15min to prepare semi-dry pug, and ageing for 4h;
(3) Molding the pug after ageing into green bodies by adopting a friction press, wherein the molding pressure is 2t/cm 2 The density of the formed green compact is 3.1-3.3g/cm 3 Then the mixture is dried after being insulated for 24h at 100 ℃ and then is sintered after being insulated for 12h at 1580 ℃ to obtain the electricityAnd melting the white corundum bricks.
The chemical composition of the products obtained in examples 1 to 10 and comparative examples 1 to 2 is shown in Table 2.
TABLE 2 chemical composition of the products obtained in examples 1-10 and comparative examples 1-2
The results of measuring physical properties of the products obtained in examples 1 to 10 and comparative examples 1 to 2 are shown in Table 3.
TABLE 3 results of measuring physical indexes of products obtained in examples 1 to 10 and comparative examples 1 to 2
As can be seen from Table 3, the homogeneous body re-sintered fused zirconia-mullite brick prepared by the invention has the porosity less than or equal to 16 percent and the volume density more than or equal to 3.00g/cm 3 The normal temperature compressive strength is more than or equal to 100MPa, the refractoriness under load temperature T of 0.2MPa 0.6 The temperature is more than or equal to 1700 ℃, the change of the re-sintering line at 1650 ℃ is less than 0.1 percent, the thermal expansion rate at 1400 ℃ is less than 0.65 percent, and the homogeneous body re-sintered fused zirconia mullite brick has good steam erosion resistance and thermal shock resistance of a glass kiln, wherein the performance of the homogeneous body re-sintered fused zirconia mullite brick prepared in the embodiment 1 is optimal. The products prepared in the comparative examples 1-2 have higher porosity and poor steam erosion resistance and thermal shock resistance of the glass kiln.
Claims (7)
1. A homogeneous body re-sintered electric smelting zirconium mullite brick is characterized in that: the aggregate component and the matrix component are zirconium mullite mineral phases and are prepared from the following powder materials, cellulose dry powder and magnesium lignosulfonate stock solution in percentage by weight:
the content of the cellulose dry powder is 0.1-0.3% of the total weight of the powder;
the content of the magnesium lignosulphonate stock solution is 2-5% of the total weight of the powder;
the physical and chemical indexes of the fused zirconia mullite in the raw materials are as follows: zrO (ZrO) 2 ：30-35％，Al 2 O 3 ：42-49％，SiO 2 ：16-20％，Fe 2 O 3 Not less than 0.3 percent and the volume density not less than 3.5g/cm 3 The apparent porosity is less than or equal to 5 percent, the mullite phase is more than or equal to 50 percent, the baddeleyite phase is more than or equal to 28 percent, the corundum phase is less than or equal to 5 percent, and the glass phase is less than or equal to 5 percent;
the preparation method comprises the following steps:
(1) Mixing fused zirconia mullite with the grain diameter of more than 1mm and less than or equal to 3mm and the grain diameter of more than 0.1mm and less than or equal to 1mm for 5-10min, adding a magnesium lignosulfonate stock solution, and mixing and grinding for 5-10min to obtain mixed coarse powder;
(2) Mixing and grinding the raw material with the particle size of less than or equal to 0.045mm and cellulose for 3-10min to obtain mixed fine powder;
(3) Adding the mixed fine powder into the mixed coarse powder, mixing and grinding for 15-20min to obtain semi-dry pug, and ageing for 4-5h;
(4) Molding the pug after ageing into green bodies with the molding pressure of 1.5-3t/cm 2 Then drying and sintering to obtain a homogeneous body, and sintering the fused zirconia-mullite brick;
the physical and chemical indexes of the homogeneous body re-sintered fused zirconia mullite brick are as follows: al (Al) 2 O 3 ：47-55％，Fe 2 O 3 ≤0.2％，ZrO 2 ：27-32％，SiO 2 :15-20%, impurity content less than 0.9%, porosity less than or equal to 16%, volume density more than or equal to 3.00g/cm 3 The normal temperature compressive strength is more than or equal to 100MPa, the 0.2MPa refractoriness under load temperature T 0.6 More than or equal to 1700 ℃, the change of the dead burning line at 1650 ℃ is less than 0.1 percent, and the thermal expansion rate at 1400 ℃ is less than 0.65 percent.
2. The homogeneous body resintered electrofused zirconium mullite brick of claim 1, wherein: physicochemical index of electro-fused white corundumComprises the following steps: al (Al) 2 O 3 ≥99.5％，Fe 2 O 3 ≤0.1％，Na 2 O≤0.35％。
3. The homogeneous body resintered electrofused zirconium mullite brick of claim 1, wherein: the physicochemical indexes of 65 zircon powder are as follows: zrO (ZrO) 2 ≥65％，Fe 2 O 3 ≤0.1％；Al 2 O 3 ≤0.4％。
4. The homogeneous body resintered electrofused zirconium mullite brick of claim 1, wherein: the physicochemical indexes of Suzhou soil are as follows: al (Al) 2 O 3 ≥36％，Fe 2 O 3 Less than or equal to 0.4 percent, less than or equal to 2 percent of impurity content and less than or equal to 15 percent of ignition loss.
5. The homogeneous body resintered fused zirconia mullite brick of claim 1, wherein: in the step (4), a friction press or a hydraulic press is adopted for forming, and the density of the formed green body is 3.1-3.3g/cm 3 。
6. The homogeneous body resintered electrofused zirconium mullite brick of claim 1, wherein: in the step (4), the drying temperature is 80-120 ℃ and the time is 24-48h.
7. The homogeneous body resintered fused zirconia mullite brick of claim 1, wherein: the sintering temperature is 1500-1600 ℃ and the time is 6-12h.
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| CN107089835A (en) * | 2017-05-03 | 2017-08-25 | 河南瑞泰耐火材料科技有限公司 | Carbon calciner andalusite mullite composite brick and preparation method thereof |
| FR3074909B1 (en) * | 2017-12-11 | 2022-03-04 | Saint Gobain Ct Recherches | METHOD FOR IDENTIFYING THE CLASS OF ELECTROFONDED AZS REFRACTORY GENERATING "STONES" IN A GLASS PRODUCT |
| CN109053176B (en) * | 2018-08-31 | 2021-10-01 | 广州市石基耐火材料厂 | Chromium-containing mullite refractory material and preparation method thereof |
| CN109336575A (en) * | 2018-10-26 | 2019-02-15 | 淄博工陶耐火材料有限公司 | One kind re-sintering electric cast mullite brick and preparation method thereof containing zirconium |
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| CN101607825A (en) * | 2008-12-30 | 2009-12-23 | 淄博工陶耐火材料有限公司 | Fused high-iron ferriporphyrin mullite recombined high-dense brick and method for making thereof |
| CN104446572A (en) * | 2014-12-23 | 2015-03-25 | 山东万乔集团有限公司 | Corundum mullite brick for high-temperaturehigh sulfur petroleum cokecalcining furnace |
| CN108727040A (en) * | 2017-04-17 | 2018-11-02 | 维苏威美国公司 | Porous refractory mould material and application thereof and manufacture |
| CN110746180A (en) * | 2019-11-25 | 2020-02-04 | 浙江自立高温科技股份有限公司 | Sintered aluminum-chromium-zirconium sliding plate brick for copper smelting anode furnace and preparation method thereof |
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