Preparation process of wear-resistant and alkali-resistant castable
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- CHANGSHA HENGAN ENG TECH CO LTD
- Filing Date
- 2024-10-08
- Publication Date
- 2026-08-07
AI Technical Summary
[0003]传统上这类性能的浇注料通常由耐火水泥材料以及一定比例的耐碱性增强剂组成,通过精心配比和科学工艺制备以达到最佳效果,然而,随着工业生产对材料性能要求的不断提高,现有技术在满足极端工况下的应用时仍存在一些未解决的问题
[0028]本发明方法通过电熔刚玉颗粒的高硬度和涂层的增强作用,显著提升了材料的耐磨性;通过莫来石片的耐碱性能和涂层的协同作用,增强了其抵御碱性腐蚀的能力,尤其是表层的防护效果;通过干混、湿法混炼和振动成型等多步骤处理,确保了原材料的均匀分散和浇注料的致密性,减少了内部气孔,提高了材料的结构稳定性和抗热震性;利用预热处理和分段升温保温,有效控制了材料的热应力,促进了涂层与基体的结合,提高了浇注料的高温性能和使用寿命;通过溶胶-凝胶涂层技术的使用,不仅增强了颗粒和薄片的表面性能,还利用热处理形成了均匀稳定的涂层,改善了材料的界面结合,提升了整体性能;通过上述工艺,浇注料在保持良好耐磨耐碱性能的同时,也提升了抗裂性和结构稳定性,从而延长了材料在恶劣环境中的使用寿命,加强浇注料表面的耐磨性能。
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Abstract
Description
Technical Field
[0001] This invention relates to the field of castable preparation technology, specifically to a preparation process for a wear-resistant and alkali-resistant castable. Background Technology
[0002] Wear-resistant and alkali-resistant castables are high-performance inorganic non-metallic materials widely used in high-temperature equipment in industries such as chemical, metallurgy, power, and building materials. Especially in environments where alkaline media are handled, their excellent wear resistance and alkali resistance make them indispensable protective materials.
[0003] Traditionally, castables of this type are usually composed of refractory cement materials and a certain proportion of alkali-resistant reinforcing agents. They are prepared through careful proportioning and scientific processes to achieve the best results. However, as industrial production continues to increase the requirements for material performance, existing technologies still have some unresolved problems in meeting the needs of applications under extreme working conditions.
[0004] Improving the alkali resistance of materials often leads to a decrease in wear resistance, and vice versa. How to improve the wear resistance of castables while ensuring their alkali resistance to adapt to more complex usage environments is a major challenge for current technology. In addition, the structure of castables is prone to change at high temperatures, leading to a decrease in performance. Especially under conditions of large temperature fluctuations, the stability of materials has become a key factor affecting their service life. Summary of the Invention
[0005] To address the aforementioned problems, this invention provides a preparation process for wear-resistant and alkali-resistant castables.
[0006] The technical solution of this invention is: a preparation process for wear-resistant and alkali-resistant castable, comprising the following steps:
[0007] S1. Weigh 10-18% Ca3SiO5 powder, 5-10% Ca2SiO4 powder, 5-10% refractory clay, 1-9% nano alumina powder, 2-8% gallium oxide powder, 2-4% composite modifier, and the balance high-alumina bauxite clinker by mass percentage to obtain raw material powder.
[0008] S2. The raw material powder described in S1 is introduced into a dry mixer and mixed for 15-30 minutes to ensure that the components are evenly distributed to obtain a mixture. Then, the mixture is added to a wet mixer, and water is added at a mass ratio of 40-70% of the raw material powder. The mixture is continuously mixed for 10-15 minutes to obtain a slurry. The slurry is pressed into shape using a vibration molding machine to ensure that there are no air holes inside the material to obtain a molded slurry.
[0009] S3. The molding slurry described in S2 is divided into component A and component B in a mass ratio of 2 to 3:1. 3 to 10% of the mass of fused alumina particles are taken, and after cleaning, the fused alumina particles are soaked in sol treatment solution A. After standing for 3 to 15 minutes, they are taken out and then dried in an oven at 50 to 100°C until the sol gels to form a uniform coating. The coating particles are aged at room temperature for 24 to 30 hours to obtain coated particles. Then, the coated particles are heat-treated and stirred evenly with component A to obtain the first main material.
[0010] Take mullite flakes accounting for 3-10% of component B by mass, wash the mullite flakes and soak them in sol treatment solution B. After standing for 3-10 minutes, take them out and then heat dry them in an oven at 50-100℃ until the sol gels to form a uniform coating. Aging at room temperature for 24-30 hours yields a coated sheet. Then heat treat it and mix the heat-treated coated sheet with component B to obtain the second main material.
[0011] S4. After mixing the first main material and the second main material described in S3, preheat the mixture, then raise the temperature to 800-850°C at a heating rate of 5-7°C / min, hold for 2-4 hours, and finally raise the temperature to 1100-1250°C at a heating rate of 2-4°C / min, hold for 2-4 hours to obtain wear-resistant and alkali-resistant castable.
[0012] Explanation: The first main material, containing coated fused corundum particles, has a higher density and sinks to the bottom of the castable, enhancing the wear resistance of the area in contact with the working surface. The second main material, containing coated mullite flakes, has a lower density and floats to the surface, improving the surface's alkali resistance and corrosion resistance. This layered structure effectively strengthens the material's protective performance under complex working conditions. This preparation process, through optimized material selection, processing methods, and heat treatment parameters, effectively enhances the performance of wear-resistant and alkali-resistant castables, making them highly effective in industrial applications, especially in environments where they need to withstand both wear and alkaline corrosion.
[0013] Further, the high-alumina bauxite clinker in S1 has an Al2O3 content of 85-90% and a particle size of 1-3 mm; the nano-alumina powder has a particle size of 30-50 nm; the refractory clay has a particle size of 0.01-0.05 mm; and the gallium oxide powder has a particle size of 45-55 μm.
[0014] Explanation: The high Al2O3 content of high-alumina bauxite clinker ensures the material's high melting point and chemical stability, especially exhibiting excellent performance in alkaline environments. It resists alkali metal corrosion. The particle size of 1-3mm provides good particle size distribution, enhancing the structural strength and thermal shock resistance of the castable, while also improving its permeability and thermal stability. The extremely fine particle size of nano-alumina powder fills tiny pores, increasing the density and hardness of the castable, significantly improving its wear resistance and corrosion resistance. Nano-alumina powder can also improve the interfacial bonding with other components, enhancing... The overall mechanical properties and crack resistance of the material are enhanced by the fine particle size of the refractory clay, which helps to form a denser microstructure, reduces porosity, and improves the material's density and corrosion resistance. As a binder, the refractory clay strengthens the bonding force between the components of the castable, improving the material's structural stability and wear resistance. The moderate particle size of the gallium oxide powder maintains good dispersibility while avoiding sedimentation problems caused by excessive fineness, which helps to form a uniform composite material structure. The addition of gallium oxide powder can improve the alkali resistance of the castable, especially under high temperature conditions, effectively resisting the corrosion of alkaline substances.
[0015] Furthermore, the Ca3SiO5 powder in S1 has two particle sizes: 5-7 μm and 35-45 μm, with a mass ratio of 1:9 between the two particle sizes; the Ca2SiO4 powder has two particle sizes: 4-6 μm and 30-40 μm, with a mass ratio of 1:6-8 between the two particle sizes.
[0016] Explanation: By mixing Ca3SiO5 and Ca2SiO4 powders of different particle sizes, a denser and more uniform microstructure can be formed. Fine-grained powder fills the voids between coarse-grained powders, reducing porosity and enhancing the material's density and wear resistance. A reasonable particle size distribution improves the material's rheological properties, making the castable easier to flow and compact during molding, thus improving molding quality and efficiency. Fine powder helps improve slurry fluidity, while coarse powder helps increase structural strength. Mixing powders of different particle sizes can enhance the mechanical properties of the castable, such as compressive and flexural strength. A certain ratio of fine and coarse powder can optimize the stress distribution of the material, improving its impact resistance and crack resistance. Ca3SiO5 and Ca2SiO4 powders act as chemical stabilizers in the castable; by controlling the particle size ratio, the material's alkali resistance and corrosion resistance can be enhanced. Fine powder is more readily involved in chemical reactions, improving the material's chemical activity and durability.
[0017] Furthermore, the composite modifier described in S1 consists of 15-35 wt% silane coupling agent and the balance being nano-silica.
[0018] Explanation: Silane coupling agents can form chemical bonds between inorganic materials such as nano-silica and organic materials in castables, significantly improving the interfacial adhesion between the two, thereby enhancing the overall structural strength and durability of the castable. The high specific surface area and surface energy of nano-silica often lead to its agglomeration in organic media. The use of silane coupling agents can effectively reduce this agglomeration, improve the dispersibility of nanoparticles in the castable matrix, and thus improve the uniformity and performance of the material. Nano-silica particles modified with silane coupling agents can be better dispersed in the castable. These particles can form a reinforced network structure on the material surface, improving the wear resistance and chemical corrosion resistance of the castable.
[0019] Furthermore, the particle size of the fused alumina particles is 1-8 mm; the average length and width of the mullite flakes are 0.5-2 mm, and the thickness is 0.5-1.5 mm.
[0020] Explanation: Due to their high hardness and wear resistance, fused alumina particles can significantly improve the wear resistance of castables. The particle size range of 1-8mm can form multi-layer protection, effectively resisting wear. Mullite flakes can form a dense protective layer on the surface of the castable, improving alkali resistance and corrosion resistance. The ratio of components A to B ensures the sinking of fused alumina particles and the floating of mullite flakes, forming a reasonable structural distribution, that is, high wear resistance and high alkali resistance materials are located on the surface, maximizing performance. The large particle size of fused alumina combined with mullite flakes can reduce the porosity inside the castable, improving the compactness and stability of the structure.
[0021] Further, the preparation method of the sol treatment solution A in S3 is as follows: by mass percentage, at room temperature, 10-20% TEOS, 10-20% deionized water, 1-5% ammonia water and the balance ethanol are mixed and stirred until the solution is clear to obtain sol treatment solution A; the preparation method of the sol treatment solution B is as follows: by mass percentage, at room temperature, 10-20% Zr(OC2H5)4, 10-20% deionized water, 1-5% nitric acid and the balance ethanol are mixed and stirred until the solution is clear to obtain sol treatment solution B.
[0022] Explanation: Sol-gel technology can prepare uniform and highly adhesive coatings because the sol can penetrate into the tiny pores of the material, forming a continuous and uniform coating, thus improving the surface properties of the material; TEOS (tetraethoxysilane) undergoes hydrolysis and condensation under the catalysis of ammonia to form a silica coating with high chemical stability, enhancing the wear resistance and corrosion resistance of fused alumina particles; Zr(OC2H5)4 (tetraethoxyzirconium) forms a zirconium oxide coating under the catalysis of nitric acid, which improves the high-temperature resistance and alkali resistance of mullite flakes; the high bonding strength between the sol-gel coating and the substrate material effectively improves interfacial bonding, reduces stress concentration at the interface, and improves the overall mechanical properties of the material.
[0023] Further, the heat treatment method for the coating particles in S3 is as follows: pre-calcining the coating particles at 400–600°C for 1–2 hours to remove organic matter from the sol. Then, calcining the coating particles at 1000–1200°C for 2–4 hours; the heat treatment method for the coating sheet is as follows: pre-calcining the coating sheet at 400–600°C for 1–2 hours to remove organic matter from the sol. Then, calcining the coating sheet at 1200–1400°C for 2–4 hours.
[0024] Note: During the pre-calcination stage at 400–600℃, residual organic matter in the sol-gel treatment solution can be effectively removed, preventing the formation of pores or cracks during subsequent high-temperature treatment, thus ensuring the integrity of the coating and the density of the material. During the calcination process of fused corundum particles at 1000–1200℃, the bonding force between the coating and the substrate material is further enhanced, improving the chemical stability and wear resistance of the coating. At the calcination temperature of 1200–1400℃, the crystal phase transformation of the coating material is completed, forming a more stable crystal phase structure, improving high-temperature resistance and alkali resistance.
[0025] Furthermore, the preheating treatment method described in S4 is as follows: the first main material and the second main material are heated from room temperature to 90-100°C at a heating rate of 9-12°C / min, and then kept at that temperature for 1-2 hours.
[0026] Note: Preheating can reduce the thermal stress generated in the material during subsequent high-temperature processing because the temperature change of the material during heating and cooling is more gradual, which helps to improve the overall stability of the molded body. Preheating can also more effectively remove moisture and organic matter from the material, reduce porosity and defects during sintering, thereby improving the density and mechanical properties of the final product.
[0027] The beneficial effects of this invention are:
[0028] This invention significantly improves the wear resistance of materials through the high hardness of fused alumina particles and the reinforcing effect of the coating; the synergistic effect of the alkali resistance of mullite flakes and the coating enhances its ability to resist alkaline corrosion, especially the surface protection effect; through multiple steps such as dry mixing, wet mixing, and vibration molding, the uniform dispersion of raw materials and the density of the castable are ensured, internal porosity is reduced, and the structural stability and thermal shock resistance of the material are improved; by using preheating treatment and segmented heating and holding, the thermal stress of the material is effectively controlled, promoting the bonding between the coating and the substrate, and improving the high-temperature performance and service life of the castable; through the use of sol-gel coating technology, not only are the surface properties of particles and flakes enhanced, but also a uniform and stable coating is formed by heat treatment, improving the interfacial bonding of the material and enhancing the overall performance; through the above processes, the castable maintains good wear and alkali resistance while also improving crack resistance and structural stability, thereby extending the service life of the material in harsh environments and strengthening the wear resistance of the castable surface. Detailed Implementation
[0029] Example 1: A preparation process for a wear-resistant and alkali-resistant castable, comprising the following steps:
[0030] S1. Weigh out 14% Ca3SiO5 powder, 7.5% Ca2SiO4 powder, 7.5% refractory clay, 5% nano alumina powder, 5% gallium oxide powder, 3% composite modifier, and the remainder high-alumina bauxite clinker by mass percentage to obtain raw material powder.
[0031] The high-alumina bauxite clinker has an Al2O3 content of 87.5% and a particle size of 2–2.5 mm; the nano-alumina powder has a particle size of 36–40 nm; the refractory clay has a particle size of 0.02–0.03 mm; and the gallium oxide powder has a particle size of 48–50 μm.
[0032] The Ca3SiO5 powder has two particle sizes: 6-6.5 μm and 38-40 μm, with a mass ratio of 1:9; the Ca2SiO4 powder has two particle sizes: 5-5.5 μm and 35-37 μm, with a mass ratio of 1:7.
[0033] The composite modifier consists of: 25 wt% silane coupling agent and the balance being nano-silica;
[0034] S2. The raw material powder described in S1 is introduced into a dry mixer and mixed for 22.5 minutes to ensure that the components are evenly distributed and a mixture is obtained. Then, the mixture is added to a wet mixer and water is added at a mass ratio of 55% of the raw material powder. The mixture is continuously mixed for 12.5 minutes to obtain a slurry. The slurry is pressed into shape using a vibration molding machine to ensure that there are no air holes inside the material and a molded slurry is obtained.
[0035] S3. The molding slurry described in S2 is divided into component A and component B in a mass ratio of 2.5:1. 6.5% of the fused alumina particles in component A are taken, cleaned and soaked in sol treatment solution A. After standing for 9 minutes, they are taken out and then dried in an oven at 75°C until the sol gels to form a uniform coating. The coating particles are aged at room temperature for 27 hours to obtain coated particles. Then, heat treatment is performed. The heat-treated coated particles are stirred evenly with component A to obtain the first main material.
[0036] Take 6.5% mullite flakes of component B by mass, wash the mullite flakes and soak them in sol treatment solution B. After standing for 6.5 minutes, take them out and dry them in an oven at 75°C until the sol gels and forms a uniform coating. Aging at room temperature for 27 hours yields a coated sheet. Then heat-treat the coated sheet and mix it evenly with component B to obtain the second main material.
[0037] The fused alumina particles have a particle size of 4.5–5 mm; the mullite flakes have an average length and width of 1–1.5 mm and a thickness of 1–1.2 mm.
[0038] The preparation method of the sol-gel treatment solution A is as follows: by mass percentage, at room temperature, 15% TEOS, 15% deionized water, 2.5% ammonia water, and the balance ethanol are mixed and stirred until the solution is clear to obtain sol-gel treatment solution A; the preparation method of the sol-gel treatment solution B is as follows: by mass percentage, at room temperature, 15% Zr(OC2H5)4, 15% deionized water, 2.5% nitric acid, and the balance ethanol are mixed and stirred until the solution is clear to obtain sol-gel treatment solution B;
[0039] The heat treatment method for the coating particles is as follows: the coating particles are pre-calcined at 500℃ for 1.5 hours to remove organic matter from the sol. Then, the coating particles are calcined at 1100℃ for 3 hours. The heat treatment method for the coating sheet is as follows: the coating sheet is pre-calcined at 500℃ for 1.5 hours to remove organic matter from the sol. Then, the coating sheet is calcined at 1300℃ for 3 hours.
[0040] S4. After mixing the first main material and the second main material described in S3, the mixture is preheated, then heated to 825°C at a heating rate of 6°C / min and held for 3 hours. Finally, the mixture is heated to 1200°C at a heating rate of 3°C / min and held for 3 hours to obtain wear-resistant and alkali-resistant castable.
[0041] The preheating treatment method is as follows: the first main material and the second main material are heated from room temperature to 95°C at a heating rate of 10.5°C / min, and then kept at that temperature for 1.5 hours.
[0042] Example 2: The difference between this example and Example 1 is that 10% Ca3SiO5 powder, 5% Ca2SiO4 powder, 5% refractory clay, 1% nano alumina powder, 2% gallium oxide powder, 2% composite modifier, and the remainder high-alumina bauxite clinker are weighed to obtain raw material powder.
[0043] Example 3: The difference between this example and Example 1 is that 18% Ca3SiO5 powder, 10% Ca2SiO4 powder, 10% refractory clay, 9% nano alumina powder, 8% gallium oxide powder, 4% composite modifier, and the remainder high-alumina bauxite clinker are weighed to obtain raw material powder.
[0044] Example 4: The difference between this example and Example 1 is that the raw material powder described in S1 is introduced into a dry mixer and mixed for 15 minutes to ensure that the components are evenly distributed and a mixture is obtained; then the mixture is added to a wet mixer and water with a mass ratio of 40% of the raw material powder is added and the mixture is continuously mixed for 10 minutes to obtain a slurry.
[0045] Example 5: The difference between this example and Example 1 is that the raw material powder described in S1 is introduced into a dry mixer and mixed for 30 minutes to ensure that the components are evenly distributed and a mixture is obtained; then the mixture is added to a wet mixer and water accounting for 70% of the mass of the raw material powder is added, and the mixture is continuously mixed for 15 minutes to obtain a slurry.
[0046] Example 6: This example differs from Example 1 in that: the molding slurry described in S2 is divided into component A and component B in a mass ratio of 2:1. 3% of the fused alumina particles in component A are taken, cleaned, and then soaked in sol treatment solution A. After standing for 3 minutes, the particles are taken out and then dried in an oven at 50°C until the sol gels to form a uniform coating. The coating particles are aged at room temperature for 24 hours to obtain the coated particles.
[0047] Example 7: This example differs from Example 1 in that: the molding slurry described in S2 is divided into component A and component B in a mass ratio of 3:1. 10% of the mass of fused alumina particles are taken, the fused alumina particles are cleaned and then soaked in sol treatment solution A. After standing for 15 minutes, they are taken out and then dried in an oven at 100°C until the sol gels to form a uniform coating. After aging at room temperature for 30 hours, coated particles are obtained.
[0048] Example 8: The difference between this example and Example 1 is that: 3% of mullite flakes of component B were taken, the mullite flakes were washed and then soaked in sol treatment solution B. After standing for 3 minutes, they were taken out and then dried in an oven at 50°C until the sol gelled to form a uniform coating. After aging at room temperature for 24 hours, a coated sheet was obtained.
[0049] Example 9: The difference between this example and Example 1 is that: mullite flakes accounting for 10% of the mass of component B are taken, the mullite flakes are washed and then soaked in sol treatment solution B, left to stand for 10 minutes and then taken out, and then heat-dried in an oven at 100°C until the sol gels to form a uniform coating. After aging at room temperature for 30 hours, a coated sheet is obtained.
[0050] Example 10: The difference between this example and Example 1 is that the first main material and the second main material described in S3 are mixed and preheated, then heated to 800°C at a heating rate of 5°C / min and held for 2 hours, and finally heated to 1100°C at a heating rate of 2°C / min and held for 2 hours to obtain wear-resistant and alkali-resistant castable.
[0051] Example 11: The difference between this example and Example 1 is that the first main material and the second main material described in S3 are mixed and preheated, then heated to 850°C at a heating rate of 7°C / min and held for 4 hours, and finally heated to 1250°C at a heating rate of 4°C / min and held for 4 hours to obtain wear-resistant and alkali-resistant castable.
[0052] Example 12: This example differs from Example 1 in that: the Ca3SiO5 powder in S1 has two particle sizes, 5-5.5μm and 35-38μm, with a mass ratio of 1:9; the Ca2SiO4 powder has two particle sizes, 4-4.5μm and 30-35μm, with a mass ratio of 1:6.
[0053] Example 13: The difference between this example and Example 1 is that the Ca3SiO5 powder in S1 has two particle sizes: 6.5-7μm and 43-45μm, with a mass ratio of 1:9; the Ca2SiO4 powder has two particle sizes: 5.5-6μm and 37-40μm, with a mass ratio of 1:8.
[0054] Example 14: This example differs from Example 1 in that: the mass ratio of component A to component B in S3 is 2:1, the particle size of the fused alumina particles is 1-2 mm, and the average length and width of the mullite flakes are 0.5-1 mm, and the thickness is 0.5-1 mm.
[0055] Example 15: This example differs from Example 1 in that: the mass ratio of component A to component B in S3 is 3:1, the particle size of the fused alumina particles is 7-8 mm, and the average length and width of the mullite flakes are 1.5-2 mm, and the thickness is 1-1.5 mm.
[0056] Example 16: This example differs from Example 1 in that: the preparation method of the sol treatment solution A in S3 is as follows: by mass percentage, at room temperature, 10% TEOS, 10% deionized water, 1% ammonia water and the balance ethanol are mixed and stirred until the solution is clear to obtain sol treatment solution A; the preparation method of the sol treatment solution B is as follows: by mass percentage, at room temperature, 10% Zr(OC2H5)4, 10% deionized water, 1% nitric acid and the balance ethanol are mixed and stirred until the solution is clear to obtain sol treatment solution B.
[0057] Example 17: This example differs from Example 1 in that: the preparation method of the sol treatment solution A in S3 is as follows: by mass percentage, at room temperature, 20% TEOS, 20% deionized water, 5% ammonia water and the balance ethanol are mixed and stirred until the solution is clear to obtain sol treatment solution A; the preparation method of the sol treatment solution B is as follows: by mass percentage, at room temperature, 20% Zr(OC2H5)4, 20% deionized water, 5% nitric acid and the balance ethanol are mixed and stirred until the solution is clear to obtain sol treatment solution B.
[0058] Example 18: This example differs from Example 1 in that: the heat treatment method for the coating particles in S3 is as follows: the coating particles are pre-calcined at 400°C for 1 hour to remove organic matter from the sol. Then, the coating particles are calcined at 1000°C for 2 hours. The heat treatment method for the coating sheet is as follows: the coating sheet is pre-calcined at 400°C for 1 hour to remove organic matter from the sol. Then, the coating sheet is calcined at 1200°C for 2 hours.
[0059] Example 19: This example differs from Example 1 in that: the heat treatment method for the coating particles in S3 is as follows: the coating particles are pre-calcined at 600°C for 2 hours to remove organic matter from the sol. Then, the coating particles are calcined at 1200°C for 4 hours. The heat treatment method for the coating sheet is as follows: the coating sheet is pre-calcined at 600°C for 2 hours to remove organic matter from the sol. Then, the coating sheet is calcined at 1400°C for 4 hours.
[0060] Comparative Example 1: Referring to Example 1, the preheating and heat treatment of the molding slurry in the radial direction of S4 are performed directly without step S3 to obtain the casting material.
[0061] Comparative Example 2: Referring to Example 1, the Ca3SiO5 powder in S1 has two particle sizes: 8-9 μm and 50-53 μm, with a mass ratio of 1:5 for both particle sizes; the Ca2SiO4 powder has two particle sizes: 7-8 μm and 45-48 μm, with a mass ratio of 1:4 for both particle sizes.
[0062] Comparative Example 3: Referring to Example 1, the mass ratio of component A and component B in S3 is 1:1, the particle size of the fused alumina particles is 0.5-1 mm, and the average length and width of the mullite flakes are 0.2-0.3 mm, and the thickness is 0.1-0.5 mm.
[0063] Comparative Example 4: Referring to Example 1, the first main material and the second main material described in S3 were mixed and preheated. Then, the temperature was increased to 900°C at a heating rate of 8°C / min and held for 6 hours. Finally, the temperature was increased to 1300°C at a heating rate of 5°C / min and held for 1 hour to obtain wear-resistant and alkali-resistant castable.
[0064] Comparative Example 5: Referring to Example 1, the preparation method of the sol treatment solution A in S3 is as follows: by mass percentage, at room temperature, 30% TEOS, 25% deionized water, 0.5% ammonia water and the balance ethanol are mixed and stirred until the solution is clear to obtain sol treatment solution A.
[0065] Comparative Example 6: Referring to Example 1, the preparation method of the sol treatment solution B is as follows: by mass percentage, at room temperature, 30% Zr(OC2H5)4, 25% deionized water, 6% nitric acid and the remainder ethanol are mixed and stirred until the solution is clear to obtain sol treatment solution B.
[0066] To investigate the wear-resistant and alkali-resistant castables produced in Examples 1, 6-17, and Control Examples 1-6, the main materials were determined according to the experimental formulas, and 19 sets of samples were prepared for testing. The test results are shown in Table 1. The specific investigation is as follows:
[0067] Table 1. Performance test results of samples from Examples 1, 6-9 and Control Example 1
[0068]
[0069] 1. Investigate the influence of process parameters for heat treatment in step S4 on the properties of castables:
[0070] As shown in Table 1, a comparison of Examples 1, 6-9 and Control Example 1 reveals that: at 110℃ for 4 hours, the strength range of Examples 1, 6-9 was 10 to 15 MPa, with Example 1 exhibiting the highest strength; Control Example 1 had the lowest strength at 10 MPa, indicating that the structural strength of Control Example 1 was relatively low in the initial stage of hardening. At 1400℃ for 4 hours, the strength of all samples significantly increased, ranging from 16 to 19 MPa. The structural density and strength of the material increase at high temperatures, with Example 1 showing the best performance and superior structural stability under high-temperature conditions. All samples exhibited high corrosion resistance in high-temperature alkaline environments, with the wear values of Examples 1, 6-9 ranging from 3.2 to 3.8 cm. 3 It exhibits good wear resistance under high temperature and alkaline conditions; the wear value of control example 1 is the highest, at 4.1 cm. 3 Compared with Example 1, the wear performance in a high-temperature alkaline environment is poor. It can be seen that the castable prepared using the process parameters of Example 1 not only has the highest initial temperature strength and high temperature strength, but also the best wear resistance.
[0071] Table 2 Performance test results of Samples from Examples 10, 11 and Control Example 4
[0072]
[0073] 2. Investigate the influence of S4 heat treatment process parameters on the properties of castables:
[0074] As shown in Table 2, a comparison of Examples 10 and 11 with Control Example 4 reveals the following: At 110°C for 4 hours, the strength of Examples 10 and Control Example 4 was 14 MPa, while the strength of Example 11 was slightly lower at 12 MPa. In the initial stage of material hardening, the strength of Example 11 was slightly lower. At high temperatures, Example 10 exhibited better structural density and strength. The strength of Example 11 was 16 MPa, lower than Example 10 but higher than Control Example 4, indicating that Example 11's performance at high temperatures was still superior to Control Example 4. All three groups of samples showed excellent corrosion resistance. The wear resistance of Examples 10 and 11 was comparable. The wear value of Control Example 4 was 3.7 cm. 3 Its wear resistance is relatively poor, which shows that the process parameters of S4 heat treatment have a certain impact on the performance of castables.
[0075] Table 3. Performance test results of samples from Examples 12 and 13 and Control Example 2.
[0076]
[0077] 3. Investigate the influence of process parameters on Ca3SiO5 powder particle size on castable properties:
[0078] As shown in Table 3, a comparison of Examples 12 and 13 and Control Example 2 reveals that: the corrosion resistance of Control Example 2 is lower than that of Examples 12 and 13; all three groups of samples exhibit excellent corrosion resistance; the abrasion values of Examples 12 and 13 are similar; and the abrasion value of Control Example 2 is 4.3 cm. 3 The wear resistance of Example 12 was higher than that of Example 12 and 13, but its wear resistance was relatively poor. Example 12 performed best in all tests, with the highest anti-segregation strength and the lowest wear value. Although the anti-segregation strength of Example 13 was slightly lower than that of Example 12, its wear resistance was comparable to that of Example 12. It can be seen that the process parameters of Ca3SiO5 powder particle size have a certain influence on the performance of castables.
[0079] Table 4. Performance test results of samples from Examples 14, 15 and Control Example 3.
[0080]
[0081] 4. Investigate the influence of process parameters on the properties of castables based on the composition of components A and B:
[0082] As shown in Table 4, a comparison of Examples 14 and 15 with Control Example 3 reveals that Example 15 exhibits the best performance in terms of anti-precipitation strength and wear resistance at high temperatures. Not only does its strength increase significantly with increasing temperature, but it also has the lowest wear value, indicating better stability and wear resistance under high temperature and alkaline conditions. All three groups of samples demonstrate excellent corrosion resistance. Compared to Control Example 3, Example 14, despite having a similar wear value, exhibits higher strength at high temperatures. Control Example 3, on the other hand, performs poorly in both anti-precipitation strength and wear resistance, particularly in terms of wear resistance, with a significantly higher wear value than Examples 14 and 15, indicating its susceptibility to damage under high temperature and alkaline conditions. This demonstrates that the process parameters of Component A and Component B have a certain impact on the performance of the castable.
[0083] Table 5. Performance test results of Examples 16 and 17 and Control Examples 5 and 6
[0084]
[0085]
[0086] 5. Investigate the effect of the mixing ratio parameters of sol-treatment solution A and sol-treatment solution B on the properties of castables.
[0087] As shown in Table 5, a comparison of Examples 16 and 17 with Control Examples 5 and 6 reveals that: Example 17 exhibits slightly higher anti-precipitation strength at high temperatures than Example 16, and its abrasion value is only slightly higher, demonstrating good high-temperature performance and wear resistance; all four groups of samples demonstrate excellent corrosion resistance; Examples 16 and 17 show superior wear resistance, especially Example 16, which has the lowest abrasion value, indicating better wear resistance; Control Examples 5 and 6 have similar initial temperature anti-precipitation strength to the example samples, but Control Example 5 exhibits the highest anti-precipitation strength at high temperatures and a relatively high abrasion value, indicating that while its performance under high-temperature conditions is strong, its wear resistance is poor; Examples 16 and 17 demonstrate good wear resistance and high-temperature anti-precipitation strength, while Control Examples 5 and 6, although having advantages in some properties, exhibit relatively poor wear resistance. This indicates that the ratio of sol-treatment solution A to sol-treatment solution B has a certain impact on the performance of the castable.
Claims
1. A preparation process for a wear-resistant and alkali-resistant castable, characterized in that, Includes the following steps: S1. Weigh out 10-18% Ca3SiO5 powder, 5-10% Ca2SiO4 powder, 5-10% refractory clay, 1-9% nano-alumina powder, 2-8% gallium oxide powder, 2-4% composite modifier, and the balance high-alumina bauxite clinker by mass percentage to obtain raw material powder; the composite modifier consists of 15-35 wt% silane coupling agent and the balance nano-silica. S2. The raw material powder described in S1 is introduced into a dry mixer and mixed for 15-30 minutes to ensure that the components are evenly distributed to obtain a mixture. Then, the mixture is added to a wet mixer, and water with a mass ratio of 40-70% of the raw material powder is added. The mixture is continuously mixed for 10-15 minutes to obtain a slurry. The slurry is pressed into shape using a vibration molding machine to ensure that there are no air holes inside the material to obtain a molded slurry. S3. The molding slurry described in S2 is divided into component A and component B in a mass ratio of 2 to 3:
1. 3 to 10% of the mass of fused alumina particles are taken, and after cleaning, the fused alumina particles are soaked in sol treatment solution A. After standing for 3 to 15 minutes, they are taken out and then dried in an oven at 50 to 100°C until the sol gels to form a uniform coating. The coating particles are aged at room temperature for 24 to 30 hours to obtain coated particles. Then, the coated particles are heat-treated and stirred evenly with component A to obtain the first main material. Take mullite flakes accounting for 3-10% of component B by mass, wash the mullite flakes and soak them in sol treatment solution B. After standing for 3-10 minutes, take them out and then heat dry them in an oven at 50-100℃ until the sol gels to form a uniform coating. Aging at room temperature for 24-30 hours yields a coated sheet. Then heat treat it and mix the heat-treated coated sheet with component B to obtain the second main material. The preparation method of the sol-gel treatment solution A is as follows: by mass percentage, at room temperature, 10-20% TEOS, 10-20% deionized water, 1-5% ammonia water, and the balance ethanol are mixed and stirred until the solution is clear to obtain sol-gel treatment solution A; the preparation method of the sol-gel treatment solution B is as follows: by mass percentage, at room temperature, 10-20% Zr(OC2H5)4, 10-20% deionized water, 1-5% nitric acid, and the balance ethanol are mixed and stirred until the solution is clear to obtain sol-gel treatment solution B; The heat treatment method for the coating particles is as follows: pre-fire the coating particles at 400~600℃ for 1~2 hours, and then calcine the coating particles at 1000~1200℃ for 2~4 hours; the heat treatment method for the coating sheet is as follows: pre-fire the coating sheet at 400~600℃ for 1~2 hours, and then calcine the coating sheet at 1200~1400℃ for 2~4 hours. S4. After mixing the first main material and the second main material described in S3, preheat the mixture, then raise the temperature to 800-850℃ at a heating rate of 5-7℃ / min, hold for 2-4 hours, and finally raise the temperature to 1100-1250℃ at a heating rate of 2-4℃ / min, hold for 2-4 hours to obtain wear-resistant and alkali-resistant castable.
2. The preparation process of the wear-resistant and alkali-resistant castable according to claim 1, characterized in that, The high-alumina bauxite clinker in S1 has an Al2O3 content of 85-90% and a particle size of 1-3 mm; the nano-alumina powder has a particle size of 30-50 nm; the refractory clay has a particle size of 0.01-0.05 mm; and the gallium oxide powder has a particle size of 45-55 µm.
3. The preparation process of the wear-resistant and alkali-resistant castable according to claim 1, characterized in that, The Ca3SiO5 powder mentioned in S1 has two particle sizes: 5~7 µm and 35~45 µm, with a mass ratio of 1:9 between the two particle sizes; the Ca2SiO4 powder has two particle sizes: 4~6 µm and 30~40 µm, with a mass ratio of 1:6~8 between the two particle sizes.
4. The preparation process of the wear-resistant and alkali-resistant castable according to claim 1, characterized in that, The fused alumina particles in S3 have a particle size of 1-8 mm; the mullite flakes have an average length and width of 0.5-2 mm and a thickness of 0.5-1.5 mm.
5. The preparation process of the wear-resistant and alkali-resistant castable according to claim 1, characterized in that, The preheating treatment method described in S4 is as follows: the first main material and the second main material are heated from room temperature to 90-100℃ at a heating rate of 9-12℃ / min, and then kept at that temperature for 1-2 hours.
Citation Information
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