CN113213956A - Magnesium aluminate spinel brick with excellent comprehensive performance and moderate price and preparation method thereof - Google Patents
Magnesium aluminate spinel brick with excellent comprehensive performance and moderate price and preparation method thereof Download PDFInfo
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- C04B35/44—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 aluminates
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- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract
The invention relates to the technical field of refractory materials, in particular to a magnesium-aluminum spinel brick with excellent comprehensive performance and moderate price and a preparation method thereof. Comprises the following raw materials in percentage by weight: 35% -70% of magnesite grains; 5 to 30 percent of magnesia fine powder; 10 to 55 percent of magnesia-alumina spinel; 2 to 6 percent of nano zinc oxide; 1.5 to 4.5 percent of phenolic resin; 1-6% of natural crystalline flake graphite; 0.1 to 5 percent of metal fiber; 1 to 5 percent of antioxidant. The invention has high-temperature thermal state strength, strong thermal shock stability, excellent comprehensive performance and moderate price.
Description
Technical Field
The invention relates to the technical field of refractory materials, in particular to a magnesium-aluminum spinel brick with excellent comprehensive performance and moderate price and a preparation method thereof.
Background
The magnesia-alumina spinel brick takes magnesia-alumina spinel as a substrate, has good thermal shock stability, can bear water cooling for 20-25 times, even higher, and has the most outstanding advantage that the magnesia-alumina spinel brick is much better than the common magnesia brick. The research shows that the magnesia-alumina brick has good thermal shock stability because magnesia-alumina spinel and periclase belong to a cubic crystal system and have the same thermal expansion along each crystal axis direction, so that the expansion and the contraction are uniform when the temperature fluctuates, and the generated thermal stress is small. The main properties of the magnesia-alumina brick are also slightly stronger than those of the magnesia brick. Because the melting point of the magnesia-alumina spinel is higher, the refractoriness under load of the magnesia-alumina brick is improved to be 1620-1690 ℃ compared with the magnesia brick. Magnesia-alumina spinel protects periclase particles from slag attack more strongly than calcibole, so that the magnesia-alumina brick has an enhanced resistance to alkaline slag and iron oxide slag than does magnesia brick. The magnesia-alumina brick has the excellent performance, so that the magnesia-alumina brick is widely used as a masonry material for the furnace top of high-temperature smelting furnaces such as open-hearth furnaces for steelmaking, copper-smelting reverberatory furnaces and the like in China, the effect of prolonging the service life of the furnaces is achieved, the large open-hearth furnace can reach about 300 furnaces, and the medium and small open-hearth furnaces are more than 1000 furnaces.
However, the existing magnesia-alumina spinel brick has the defects of high preparation cost, low high-temperature thermal state strength, poor thermal shock stability and the like. Although some of the performance deficiencies of this material can be compensated for by technical improvements: for example, the strength of the material can be improved by introducing additives to promote sintering densification, but the introduction of the additives causes the generation of high-temperature liquid phase of the material and weakens the refractoriness under load and thermal shock resistance of the magnesia-alumina spinel brick; and for example, by introducing carbon-containing or other non-oxide additives, the densification is promoted, and the thermal shock stability and the strength of the product are improved, but the magnesium-aluminum spinel brick prepared by the method is not suitable for being used under neutral/oxidizing atmosphere conditions, and the structure and the performance of the working lining surface are rapidly degraded along with the prolonging of the working time due to the existence of the non-oxide components.
Disclosure of Invention
The invention provides a magnesia-alumina spinel brick with excellent comprehensive performance and moderate price and a preparation method thereof, which are used for overcoming the defects of the prior art and improving the performance: the invention has high-temperature thermal state strength, strong thermal shock stability, excellent comprehensive performance and moderate price.
The technical scheme of the invention is realized as follows:
the magnesia-alumina spinel brick with excellent comprehensive performance and moderate price comprises the following raw materials in percentage by weight:
the metal fiber is common fiber or stainless steel fiber.
The natural crystalline flake graphite is natural, the carbon content is 90-98 wt%, and the granularity is less than or equal to 0.15 mm.
The antioxidant is one or a mixture of more than two of Al powder, Si powder, AlMg alloy powder or SiC powder, and the granularity is less than 0.088 mm.
The magnesite grain adopts sintered or electric melting MgO, including MgO with three granularity levels of 5-3 mm, 3-1 mm and <1 mm.
The fine magnesia powder is sintered or fused MgO with the granularity less than or equal to 0.088 mm.
The particle size of the magnesium aluminate spinel is 1-2 mm.
The nano zinc oxide is powder with the granularity less than 80nm, and the chemical composition requirement of ZnO is more than or equal to 95 percent.
The preparation method of the magnesia-alumina spinel brick with excellent comprehensive performance and moderate price comprises the following steps:
1) crushing the fused magnesia, and then screening to obtain three magnesia particles with the particle sizes of 5-3 mm, 3-lmm and less than lmm;
2) finely grinding the crushed and screened magnesite grains into magnesite fine powder with the granularity less than or equal to 0.088 mm;
3) uniformly mixing the antioxidant, the magnesia-alumina spinel, the nano zinc oxide and the fine magnesia powder to prepare mixed powder;
4) respectively measuring magnesite particles with different granularities according to the proportioning requirement, adding the magnesite particles, the mixed powder and the natural crystalline flake graphite into a high-speed mixing roll in sequence for low-speed mixing for 1-2 minutes, and then adding phenolic resin for low-speed mixing for 1-2 minutes to prepare pug;
5) adding metal fibers into the pug in the high-speed mixing mill, and mixing for 8-10 minutes at a high speed to uniformly distribute the metal fibers in the pug;
6) discharging pug from high-speed mixer after mixing and finishing, beating and forming in combined friction brick press to form adobes, where the maximum force of each adobe during beating is 1.0-3 t/cm2Not less than 5 times, and the green brick density after molding is 2.80-3.25 g/cm3；
7) And (3) performing heat treatment on the formed green brick at 1500-1700 ℃ for more than 5 hours to obtain the magnesia-alumina spinel brick.
Compared with the prior art, the invention has the beneficial effects that:
1) the nano zinc oxide used in the invention has very high specific surface area and reaction activity. Passing zinc oxide over Zn at high temperature2+For Mg2+Form a solid solution, produce Mg2+The vacancies can reduce the diffusion resistance, improve the diffusion speed and facilitate the formation of the magnesia-alumina spinel, so the existence of the zinc oxide can promote the formation of more in-situ magnesia-alumina spinels in the low-carbon magnesia carbon brick. And the formation of a large amount of in-situ magnesia-alumina spinel improves the ceramic bonding degree in the low-carbon magnesia carbon brick matrix, improves the high-temperature thermal state strength, and improves the high-temperature performance of the material.
2) Due to the promoting effect of the nano zinc oxide, the function of the added metal Al antioxidant is better exerted. The reason is that the metallic Al in the magnesia carbon brick reacts with C to generate Al4C3，Al4C3 is oxidized by CO to Al2O3And then reacts with MgO to form spinel. However, studies have shown that Al4C3A considerable part of the Al can not be oxidized by CO at high temperature, thereby not only influencing the full play of the metallic Al, but also leading the Al to be fully oxidized4C3The resistance to hydration of the brick is poor, thereby affecting the performance of the brick. And the promoting effect of ZnO makes Al4C3The oxidation speed of the carbon dioxide by CO is accelerated, the deposition of C in the matrix is promoted, and Al is obviously reduced4C3The residue in the brick body obviously improves and fully plays the role of oxidation resistance and high-temperature reinforcement of metal Al. Therefore, when the same content of metal Al antioxidant is used, the high-temperature oxidation resistance of the magnesia-alumina spinel brick is obviously improved by adding the nano-zinc oxide compared with that of the magnesia-alumina spinel brick without adding the nano-zinc oxide.
3) The nanometer zinc oxide can effectively fill the gaps in the material matrix at normal temperature due to small granularity, thereby improving the volume density of the material and reducing the porosity. Under the action of high temperature, the generation of a large amount of in-situ magnesia-alumina spinel is promoted, the density of the in-situ spinel is improved, and a large amount of in-situ spinel is filled among magnesia particles in a low-carbon magnesia carbon brick matrix, so that the bonding state among the magnesia particles is improved, the integral density of the material is improved, the thermal shock resistance of the material is effectively improved, the infiltration of slag can be blocked, and the erosion resistance is improved.
4) The nano zinc oxide used in the invention is a byproduct in zinc smelting, has stable and easy source and lower price compared with other oxide nano powder, and is suitable for industrial production.
5) The graphite used in the invention is natural graphite, has stable source and lower price, and is suitable for industrial production.
Detailed Description
The following further illustrates embodiments of the invention, but is not intended to limit the scope thereof:
the magnesia-alumina spinel brick with excellent comprehensive performance and moderate price comprises the following raw materials in percentage by weight:
the metal fiber is common fiber or stainless steel fiber.
The natural crystalline flake graphite is natural, the carbon content is 90-98 wt%, and the granularity is less than or equal to 0.15 mm.
The antioxidant is one or a mixture of more than two of Al powder, Si powder, AlMg alloy powder or SiC powder, and the granularity is less than 0.088 mm.
The magnesite grain adopts sintered or electric melting MgO, including MgO with three granularity levels of 5-3 mm, 3-1 mm and <1 mm.
The fine magnesia powder is sintered or fused MgO with the granularity less than or equal to 0.088 mm.
The particle size of the magnesium aluminate spinel is 1-2 mm.
The nano zinc oxide is powder with the granularity less than 80nm, and the chemical composition requirement of ZnO is more than or equal to 95 percent.
The preparation method of the magnesia-alumina spinel brick with excellent comprehensive performance and moderate price comprises the following steps:
1) crushing the fused magnesia, and then screening to obtain three magnesia particles with the particle sizes of 5-3 mm, 3-lmm and less than lmm;
2) finely grinding the crushed and screened magnesite grains into magnesite fine powder with the granularity less than or equal to 0.088 mm;
3) uniformly mixing the antioxidant, the magnesia-alumina spinel, the nano zinc oxide and the fine magnesia powder to prepare mixed powder;
4) respectively measuring magnesite particles with different granularities according to the proportioning requirement, adding the magnesite particles, the mixed powder and the natural crystalline flake graphite into a high-speed mixing roll in sequence for low-speed mixing for 1-2 minutes, and then adding phenolic resin for low-speed mixing for 1-2 minutes to prepare pug;
5) adding metal fibers into the pug in the high-speed mixing mill, and mixing for 8-10 minutes at a high speed to uniformly distribute the metal fibers in the pug;
6) discharging pug from high-speed mixer after mixing and finishing, beating and forming in combined friction brick press to form adobes, where the maximum force of each adobe during beating is 1.0-3 t/cm2Not less than 5 times, and the green brick density after molding is 2.80-3.25 g/cm3；
7) And (3) performing heat treatment on the formed green brick at 1500-1700 ℃ for more than 5 hours to obtain the magnesia-alumina spinel brick.
Example (b):
the following 5 examples are given as specific descriptions of the raw materials used in the embodiments of the present invention, and the specific contents are shown in table 1.
Table 1: examples 1 to 5, a formulation of magnesium aluminate spinel brick (weight percentage of the unit: weight%)
| Raw materials | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Magnesia particles of 1-5 mm | 25 | 30 | 35 | 40 | 50 |
| Magnesia particles less than 1mm | 10 | 15 | 15 | 15 | 20 |
| Fine magnesia powder of 0.088mm or less | 5 | 7 | 8 | 10 | 20 |
| Nano zinc oxide less than 80nm | 2 | 3 | 4 | 5 | 6 |
| Natural crystalline flake graphite is less than or equal to 0.15mm | 1 | 2 | 2 | 2 | 3 |
| Phenolic resin | 1.5 | 2 | 2 | 2 | 2 |
| Metal fiber | 0.5 | 1 | 1 | 1 | 1 |
| Antioxidant is less than or equal to 0.088mm | 1 | 1 | 1.5 | 1 | 1 |
| 1-2 mm of magnesium aluminate spinel | 10 | 15 | 30 | 20 | 35 |
The nano zinc oxide used in the invention has very high specific surface area and reaction activity. Passing zinc oxide over Zn at high temperature2+For Mg2+Form a solid solution, produce Mg2+The vacancies can reduce the diffusion resistance, improve the diffusion speed and facilitate the formation of the magnesia-alumina spinel, so the existence of the zinc oxide can promote the formation of more in-situ magnesia-alumina spinels in the low-carbon magnesia carbon brick. And the formation of a large amount of in-situ magnesia-alumina spinel improves the ceramic bonding degree in the low-carbon magnesia carbon brick matrix, improves the high-temperature thermal state strength, and improves the high-temperature performance of the material.
Due to the promoting effect of the nano zinc oxide, the function of the added metal Al antioxidant is better exerted. The reason is that the metallic Al in the magnesia carbon brick reacts with C to generate Al4C3，Al4C3 is oxidized by CO to Al2O3And then reacts with MgO to form spinel. However, studies have shown that Al4C3A considerable part of the Al can not be oxidized by CO at high temperature, thereby not only influencing the full play of the metallic Al, but also leading the Al to be fully oxidized4C3The resistance to hydration of the brick is poor, thereby affecting the performance of the brick. And the promoting effect of ZnO makes Al4C3The oxidation speed of the carbon dioxide by CO is accelerated, the deposition of C in the matrix is promoted, and Al is obviously reduced4C3The residue in the brick body obviously improves and fully plays the role of oxidation resistance and high-temperature reinforcement of metal Al. Therefore, when the same content of metal Al antioxidant is used, the high-temperature oxidation resistance of the magnesia-alumina spinel brick is obviously improved by adding the nano-zinc oxide compared with that of the magnesia-alumina spinel brick without adding the nano-zinc oxide.
The nanometer zinc oxide can effectively fill the gaps in the material matrix at normal temperature due to small granularity, thereby improving the volume density of the material and reducing the porosity. Under the action of high temperature, the generation of a large amount of in-situ magnesia-alumina spinel is promoted, the density of the in-situ spinel is improved, and a large amount of in-situ spinel is filled among magnesia particles in a low-carbon magnesia carbon brick matrix, so that the bonding state among the magnesia particles is improved, the integral density of the material is improved, the thermal shock resistance of the material is effectively improved, the infiltration of slag can be blocked, and the erosion resistance is improved.
The nano zinc oxide used in the invention is a byproduct in zinc smelting, has stable and easy source and lower price compared with other oxide nano powder, and is suitable for industrial production. The graphite used in the invention is natural graphite, has stable source and lower price, and is suitable for industrial production.
The invention has high-temperature thermal state strength, strong thermal shock stability, excellent comprehensive performance and moderate price.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. The magnesia-alumina spinel brick with excellent comprehensive performance and moderate price is characterized by comprising the following raw materials in percentage by weight:
2. the magnesia-alumina spinel brick of claim 1, wherein the metal fiber is a common fiber or a stainless steel fiber.
3. The magnesium aluminate spinel brick with excellent comprehensive performance and moderate price according to claim 1, wherein the natural crystalline flake graphite is natural, the carbon content is 90-98 wt%, and the granularity is less than or equal to 0.15 mm.
4. The magnesium aluminate spinel brick with excellent comprehensive performance and moderate price according to claim 1, wherein the antioxidant is one or a mixture of more than two of Al powder, Si powder, AlMg alloy powder or SiC powder, and the particle size is less than 0.088 mm.
5. The magnesium aluminate spinel brick with excellent comprehensive performance and moderate price according to claim 1, wherein the magnesite grain is sintered or fused MgO, and comprises MgO with three grain size grades of 5-3 mm, 3-1 mm and <1 mm.
6. The magnesia-alumina spinel brick of claim 1, wherein the fine magnesia powder is sintered or fused MgO with a particle size of 0.088mm or less.
7. The magnesia-alumina spinel brick with excellent comprehensive performance and moderate price according to claim 1, wherein the particle size of the magnesia-alumina spinel brick is 1-2 mm.
8. The magnesia-alumina spinel brick with excellent comprehensive performance and moderate price according to claim 1, wherein the nano-zinc oxide is powder with the granularity of less than 80nm, and the chemical component requirement of ZnO is more than or equal to 95 percent.
9. The method for preparing the magnesium aluminate spinel brick with excellent comprehensive performance and moderate price according to claim 1 is characterized by comprising the following steps:
1) crushing the fused magnesia, and then screening to obtain three magnesia particles with the particle sizes of 5-3 mm, 3-1 mm and less than 1 mm;
2) finely grinding the crushed and screened magnesite grains into magnesite fine powder with the granularity less than or equal to 0.088 mm;
3) uniformly mixing the antioxidant, the magnesia-alumina spinel, the nano zinc oxide and the fine magnesia powder to prepare mixed powder;
4) respectively measuring magnesite particles with different granularities according to the proportioning requirement, adding the magnesite particles, the mixed powder and the natural crystalline flake graphite into a high-speed mixing roll in sequence for low-speed mixing for 1-2 minutes, and then adding phenolic resin for low-speed mixing for 1-2 minutes to prepare pug;
5) adding metal fibers into the pug in the high-speed mixing mill, and mixing for 8-10 minutes at a high speed to uniformly distribute the metal fibers in the pug;
6) discharging pug from high-speed mixer after mixing and finishing, beating and forming in combined friction brick press to form adobes, where the maximum force of each adobe during beating is 1.0-3 t/cm2Not less than 5 times, and the green brick density after molding is 2.80-3.25 g/cm3；
7) And (3) performing heat treatment on the formed green brick at 1500-1700 ℃ for more than 5 hours to obtain the magnesia-alumina spinel brick.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115925433A (en) * | 2022-12-31 | 2023-04-07 | 海城利尔麦格西塔材料有限公司 | Forsterite composite brick and preparation method thereof |
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| CN106892647A (en) * | 2017-03-22 | 2017-06-27 | 辽宁中镁控股股份有限公司 | A kind of compound magnesia carbon brick and preparation method thereof |
| CN110143807A (en) * | 2019-05-28 | 2019-08-20 | 海城利尔麦格西塔材料有限公司 | A kind of ladle slag line metallic composite low carbon magnesium carbon brick and preparation method thereof |
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| CN101531533A (en) * | 2009-04-22 | 2009-09-16 | 济南鲁东耐火材料有限公司 | Low carbon magnesia carbon brick and preparation method thereof |
| CN101555150A (en) * | 2009-05-18 | 2009-10-14 | 郑州大学 | Low-carbon magnesia carbon brick containing nanometer zinc oxide |
| CN104478455A (en) * | 2014-12-24 | 2015-04-01 | 辽宁中镁控股股份有限公司 | Low-carbonmagnesia carbon brick with non-oxidereinforcing and toughening structure and preparation method of low-carbonmagnesia carbon brick |
| CN105036770A (en) * | 2015-07-09 | 2015-11-11 | 长兴泓矿炉料有限公司 | Magnesium-aluminum refractory material and preparation method therefor |
| CN105837229A (en) * | 2016-03-19 | 2016-08-10 | 江苏诺明高温材料股份有限公司 | Preparation method of magnesium aluminate spinel brick |
| CN106892647A (en) * | 2017-03-22 | 2017-06-27 | 辽宁中镁控股股份有限公司 | A kind of compound magnesia carbon brick and preparation method thereof |
| CN110143807A (en) * | 2019-05-28 | 2019-08-20 | 海城利尔麦格西塔材料有限公司 | A kind of ladle slag line metallic composite low carbon magnesium carbon brick and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115925433A (en) * | 2022-12-31 | 2023-04-07 | 海城利尔麦格西塔材料有限公司 | Forsterite composite brick and preparation method thereof |
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Application publication date: 20210806 |