CN115490528B - High-strength refractory brick and preparation method thereof - Google Patents
High-strength refractory brick and preparation method thereof Download PDFInfo
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- CN115490528B CN115490528B CN202211365424.9A CN202211365424A CN115490528B CN 115490528 B CN115490528 B CN 115490528B CN 202211365424 A CN202211365424 A CN 202211365424A CN 115490528 B CN115490528 B CN 115490528B
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- 239000011449 brick Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002699 waste material Substances 0.000 claims abstract description 40
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 31
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 8
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 7
- 230000032683 aging Effects 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000009740 moulding (composite fabrication) Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 9
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 8
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 8
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 8
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 8
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229910052573 porcelain Inorganic materials 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
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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
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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
- C04B35/185—Mullite 3Al2O3-2SiO2
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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Abstract
The invention discloses a high-strength refractory brick which comprises the following raw materials in parts by weight: 100 parts of main materials, 5-7 parts of aluminum powder and 4-6 parts of binder, wherein the main materials are a mixture consisting of waste electroceramics, activated alumina, nano alumina and nano silicon dioxide. The invention also discloses a preparation method of the high-strength refractory brick, which comprises the following steps: uniformly mixing the main material, aluminum powder and a binder aqueous solution, aging, press-forming, drying and sintering to obtain the high-strength refractory brick, wherein the sintering process comprises the following steps: heating to 600-620 ℃ in a nitrogen atmosphere, and preserving heat for 6-7h; then the temperature is raised to 1050-1150 ℃ and changed into air atmosphere, the temperature is continuously raised to 1300-1400 ℃, and the temperature is kept for 4-4.5h. The invention uses the waste electroceramics as the raw material of the refractory brick, can reduce the cost and avoid environmental pollution, and the refractory brick has high strength.
Description
Technical Field
The invention relates to the technical field of refractory brick materials, in particular to a high-strength refractory brick and a preparation method thereof.
Background
The electric porcelain material is widely applied in China, and a large amount of waste electric porcelain can be generated. At present, the waste electric porcelain is treated by adopting a landfill or accumulation mode. But the waste electric porcelain has extremely stable physicochemical property, strong oxidation resistance, good corrosion resistance, difficult natural degradation and pollution to the environment. Therefore, a method for recycling the waste electric porcelain is needed.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the high-strength refractory brick and the preparation method thereof.
The invention provides a high-strength refractory brick, which comprises the following raw materials in parts by weight: 100 parts of main materials, 5-7 parts of aluminum powder and 4-6 parts of binder, wherein the main materials are a mixture consisting of waste electroceramics, activated alumina, nano alumina and nano silicon dioxide.
Preferably, the weight ratio of the waste electroceramic, the activated alumina, the nano alumina and the nano silica is 90.
Preferably, the molar ratio of the aluminum oxide to the silicon oxide in the waste electric porcelain is 1.4-1.6.
The invention selects the waste electric porcelain, the active alumina, the nano alumina and the nano silica to form the main material according to proper proportion, and adjusts the molar ratio of the alumina to the silica in the waste electric porcelain, and the mullite refractory brick can be prepared by sintering, thereby improving the strength of the refractory brick.
Preferably, the particle size of the waste electric porcelain is 0.1-1mm, 0.045-0.1mm.
Preferably, the particle size of the activated alumina is < 0.045mm.
Preferably, the weight ratio of the waste electric porcelain with the grain diameter of 0.1-1mm to the waste electric porcelain with the grain diameter of 0.045-0.1mm is 3.
Preferably, the binder is carboxymethyl cellulose.
The invention also provides a preparation method of the high-strength refractory brick, which comprises the following steps: uniformly mixing the main material, aluminum powder and a binder aqueous solution, aging, press-forming, drying and sintering to obtain the high-strength refractory brick, wherein the sintering process comprises the following steps: heating to 600-620 ℃ in a nitrogen atmosphere, and preserving heat for 6-7h; then the temperature is increased to 1050-1150 ℃, the air atmosphere is changed, the temperature is continuously increased to 1300-1400 ℃, and the temperature is kept for 4-4.5h.
The temperature is kept at 600-620 ℃ for 6-7h in the nitrogen atmosphere, an AlN film can be formed on the surface of the aluminum powder, the binder becomes carbon residue, and AlN can improve the strength of the refractory brick, but the refractory brick is easy to generate hydration reaction in the natural environment to cause crushing; in order to solve the problem, the temperature is raised to 1050-1150 ℃, the aluminum powder coated by the AlN film is changed into an air atmosphere, during the temperature raising, the aluminum powder is in a high-activity molten state, when the temperature is 1050-1150 ℃, the air enters to decompose the carbon residue to form micro air holes, at the moment, the AlN film is broken, the molten aluminum overflows, the formed holes are filled, the surface of the AlN is coated, and then the aluminum oxide is generated; the porosity can be reduced, the AlN coated by the alumina can also improve the strength of the refractory brick and avoid the crushing of the AlN; then heating to 1300-1400 ℃ for sintering to further reduce the porosity and improve the strength of the refractory brick.
Preferably, the temperature is raised to 600-620 ℃ at a rate of 2-3 ℃/min.
Preferably, the temperature is raised to 1050-1150 ℃ at a rate of 4-6 ℃/min.
Preferably, the temperature is continuously increased to 1300-1400 ℃ at the speed of 4-6 ℃/min.
The proper temperature rise rate is selected to improve the density of the AlN film, reduce the pore diameter of the pores formed by volatilization of the residual carbon, further improve the sintering effect and improve the strength of the refractory brick.
Has the advantages that:
the mullite refractory brick is prepared by matching the waste electric porcelain with the activated alumina, the nano alumina and the nano silica in a proper proportion, so that the strength of the refractory brick is improved, and the waste electric porcelain is used as a raw material, so that the cost is reduced, and the environmental pollution is avoided;
the strength of the invention can be greatly improved by adding a proper amount of aluminum powder and combining a proper sintering procedure; and proper amount of nano alumina and nano silica are added to be matched with each other in the sintering process, so that the aperture can be further refined, the porosity is reduced, and the strength of the refractory brick is improved.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
A high-strength refractory brick comprises the following raw materials in parts by weight: 90g of waste electric porcelain, 6g of activated alumina with the particle size less than 0.045mm, 2g of nano alumina, 2g of nano silica, 5g of aluminum powder and 4g of carboxymethyl cellulose;
wherein, the molar ratio of alumina to silica in the waste electric porcelain is 1.6;
the particle size of the waste electric porcelain is 0.1-1mm and 0.045-0.1mm;
the weight ratio of the waste electric porcelain with the grain diameter of 0.1-1mm to the waste electric porcelain with the grain diameter of 0.045-0.1mm is 3;
the preparation method of the high-strength refractory brick comprises the following steps: uniformly mixing waste electroceramics, activated alumina, nano silicon dioxide, aluminum powder and a carboxymethyl cellulose aqueous solution, aging at room temperature for 24 hours, press-forming at 20MPa, drying at room temperature for 24 hours, drying at 110 ℃ for 24 hours, and sintering to obtain the high-strength refractory brick, wherein the sintering process comprises the following steps: heating to 620 ℃ at the speed of 3 ℃/min in the nitrogen atmosphere, preserving heat for 6h, then slowly introducing air to convert into the air atmosphere when heating to 1150 ℃ at the speed of 6 ℃/min, then continuously heating to 1400 ℃ at the speed of 6 ℃/min, and preserving heat for 4h.
Example 2
A high-strength refractory brick comprises the following raw materials in parts by weight: 90g of waste electric porcelain, 7g of activated alumina with the particle size less than 0.045mm, 1.5g of nano alumina, 1.5g of nano silicon dioxide, 7g of aluminum powder and 6g of carboxymethyl cellulose;
wherein, the molar ratio of alumina to silica in the waste electric porcelain is 1.4;
the particle size of the waste electric porcelain is 0.1-1mm and 0.045-0.1mm;
the weight ratio of the waste electric porcelain with the grain diameter of 0.1-1mm to the waste electric porcelain with the grain diameter of 0.045-0.1mm is 3;
the preparation method of the high-strength refractory brick comprises the following steps: uniformly mixing waste electroceramics, activated alumina, nano silicon dioxide, aluminum powder and a carboxymethyl cellulose aqueous solution, aging at room temperature for 24 hours, press-forming at 20MPa, drying at room temperature for 24 hours, drying at 110 ℃ for 24 hours, and sintering to obtain the high-strength refractory brick, wherein the sintering process comprises the following steps: heating to 600 ℃ at the speed of 2 ℃/min in the nitrogen atmosphere, preserving heat for 7h, then slowly introducing air to convert into the air atmosphere when heating to 1050 ℃ at the speed of 4 ℃/min, then continuously heating to 1300 ℃ at the speed of 4 ℃/min, and preserving heat for 4.5h.
Example 3
A high-strength refractory brick comprises the following raw materials in parts by weight: 90g of waste electric porcelain, 7g of activated alumina with the particle size less than 0.045mm, 1.5g of nano alumina, 1.5g of nano silicon dioxide, 6g of aluminum powder and 5g of carboxymethyl cellulose;
wherein the molar ratio of aluminum oxide to silicon oxide in the waste electric porcelain is 1.5;
the particle size of the waste electroceramics is 0.1-1mm and 0.045-0.1mm;
the weight ratio of the waste electric porcelain with the grain diameter of 0.1-1mm to the waste electric porcelain with the grain diameter of 0.045-0.1mm is 3;
the preparation method of the high-strength refractory brick comprises the following steps: uniformly mixing waste electroceramics, activated alumina, nano silicon dioxide, aluminum powder and a carboxymethyl cellulose aqueous solution, aging at room temperature for 24 hours, performing compression molding at 20MPa, drying at room temperature for 24 hours, drying at 110 ℃ for 24 hours, and sintering to obtain the high-strength refractory brick, wherein the sintering process comprises the following steps: heating to 610 deg.C at a speed of 2.5 deg.C/min in nitrogen atmosphere, maintaining for 6.5h, heating to 1100 deg.C at a speed of 5 deg.C/min, slowly introducing air to convert into air atmosphere, heating to 1350 deg.C at a speed of 5 deg.C/min, and maintaining for 4.5h.
Comparative example 1
The sintering procedure is as follows: the temperature was raised to 610 ℃ at a rate of 2.5 ℃/min in the air atmosphere, and the temperature was maintained for 6.5 hours, and then raised to 1350 ℃ at a rate of 5 ℃/min, and the temperature was maintained for 4.5 hours, otherwise the same as in example 3.
Comparative example 2
The same procedure as in example 3 was repeated, except that no powdery aluminum was contained.
Comparative example 3
The process is the same as example 3 except that the nano alumina and the nano silica are not contained.
The firebricks obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to a performance test, and the results are shown in Table 1.
TABLE 1 test results
| Detecting items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Porosity% | 13.0 | 14.2 | 13.5 | 40.3 | 26.5 | 14.9 |
| Tensile strength MPa at 1400 DEG C | 54 | 51 | 55 | 19 | 30 | 48 |
As can be seen from the results of table 1, the present invention has good strength.
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 as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (7)
1. The high-strength refractory brick is characterized by comprising the following raw materials in parts by weight: 100 parts of main materials, 5-7 parts of aluminum powder and 4-6 parts of binder, wherein the main materials are a mixture consisting of waste electroceramics, activated alumina, nano alumina and nano silicon dioxide;
the weight ratio of the waste electroceramic to the activated alumina to the nano silica is 90-7;
the molar ratio of alumina to silica in the waste electroceramics is 1.4-1.6;
the binder is carboxymethyl cellulose;
the preparation method of the high-strength refractory brick comprises the following steps: uniformly mixing the main material, aluminum powder and a binder aqueous solution, aging, press-forming, drying and sintering to obtain the high-strength refractory brick, wherein the sintering process comprises the following steps: heating to 600-620 ℃ in a nitrogen atmosphere, and preserving heat for 6-7h; then the temperature is increased to 1050-1150 ℃, the air atmosphere is changed, the temperature is continuously increased to 1300-1400 ℃, and the temperature is kept for 4-4.5h.
2. The high-strength refractory brick according to claim 1, wherein the grain size of the waste electroceramics is 0.1-1mm, 0.045-0.1mm.
3. The high strength refractory brick as claimed in claim 1 or claim 2, wherein the activated alumina has a particle size of < 0.045mm.
4. The high-strength refractory brick according to claim 2, wherein the weight ratio of the waste electroceramics with the grain size of 0.1-1mm to the waste electroceramics with the grain size of 0.045-0.1mm is 3.
5. The high strength refractory brick as claimed in claim 1 or 2, wherein the temperature is raised to 600-620 ℃ at a rate of 2-3 ℃/min.
6. The high strength refractory brick as claimed in claim 1 or 2, wherein the temperature is raised to 1050-1150 ℃ at a rate of 4-6 ℃/min.
7. The high strength refractory brick as claimed in claim 1 or 2, wherein the temperature is further raised to 1300-1400 ℃ at a rate of 4-6 ℃/min.
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| CN202211365424.9A CN115490528B (en) | 2022-10-31 | 2022-10-31 | High-strength refractory brick and preparation method thereof |
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| CN202211365424.9A CN115490528B (en) | 2022-10-31 | 2022-10-31 | High-strength refractory brick and preparation method thereof |
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| CN115490528A CN115490528A (en) | 2022-12-20 |
| CN115490528B true CN115490528B (en) | 2023-04-18 |
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| CN105060905B (en) * | 2015-07-24 | 2018-01-05 | 瑞泰科技股份有限公司 | Low alkaline-resisting mullite brick of aluminium and preparation method thereof |
| CN107473719A (en) * | 2017-08-24 | 2017-12-15 | 浙江科屹耐火材料有限公司 | A kind of low carbon high-strength refractory material and its preparation technology |
| CN112374896B (en) * | 2020-11-12 | 2022-05-27 | 广东工业大学 | Slurry of high-performance aluminum nitride ceramic substrate and preparation method thereof |
| CN112573896A (en) * | 2020-12-25 | 2021-03-30 | 唐山北方瓷都陶瓷集团卫生陶瓷有限责任公司 | High-strength ceramic biscuit and preparation method thereof |
| CN113105222B (en) * | 2021-04-07 | 2023-03-28 | 重庆丰淼生态环境科技有限责任公司 | Method for preparing mullite by using aluminum ash |
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