Preparation method of high-strength sintered tile

Abstract

The invention belongs to the technical field of building materials, and particularly relates to a preparation method of a high-strength sintered tile. The preparation method of the high-strength sintered tile comprises the following steps: (1) crushing green body raw materials, sieving, adding water, carrying out ball milling, and carrying out spray drying to obtain powder; (2) performing compression molding on the powder obtained in the step (1) to obtain a green body; drying the green body to obtain a tile blank; (3) coating the tile blank obtained in the step (2) with glaze, and drying to obtain a glazed tile blank; and sintering the glazed tile blank, and then cooling to room temperature to obtain the ceramic tile. The high-strength sintered tile obtained by the preparation method is high in bending strength, high in thermal stability, low in water absorption and good in freezing resistance, and has a wide application prospect.

Description

Technical Field

[0001] The invention belongs to the field of building materials, and particularly relates to a method for preparing high-strength sintered tiles. Background Art

[0002] Sintered tiles are ceramic tiles made through a high-temperature sintering process. They are commonly used for roof coverings and floor paving. With the development of modern industry, the raw materials for sintered tiles are also being utilized in a waste-based resource-based manner, such as the production of sintered tiles from mining waste. However, mining waste contains a large number of impurities and unstable mineral components, which may not form a dense structure during the sintering process, thus affecting the flexural strength of the sintered tiles. Furthermore, the thermal expansion coefficients of different mineral components in mining waste vary significantly, which can easily induce stress within the tiles during temperature fluctuations, affecting the thermal stability of the sintered tiles. Furthermore, the pores within the mining waste raw material components are numerous and fail to fully close during the sintering process, resulting in high water absorption. When these highly absorbent sintered tiles freeze, the expansion of water exerts pressure on the internal structure of the tiles, causing them to crack. Therefore, further research is needed to investigate the methods of producing high-strength sintered tiles from mining waste, based on their strength, thermal stability, water absorption, and frost resistance.

[0003] Based on the above purpose, the present invention provides a method for preparing a high-strength sintered tile. Summary of the Invention

[0004] The first object of the present invention is to provide a method for preparing high-strength sintered tiles.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is: A method for preparing a high-strength sintered tile comprises the following steps: (1) Ball milling and powder making: the green body raw materials are crushed and sieved, and then water and a water reducer are added for ball milling, and then spray dried after ball milling to obtain a powder; the green body raw materials include the following components by weight: 50-60 parts of mine waste, 10-20 parts of bentonite, 15-20 parts of clay, 10-20 parts of potassium feldspar, 5-10 parts of quartz, and 5-10 parts of modified silicon carbide fiber; (2) Molding and drying: the powder obtained in step (1) is pressed into a green body; the green body is dried to obtain a green tile; (3) Glazing and firing: applying a glaze to the green tile obtained in step (2), and drying the green tile to obtain a glazed green tile; sintering the glazed green tile, and then cooling it to room temperature to obtain a green tile; the glaze comprises the following components in parts by weight: 30-40 parts of nano-silicon dioxide, 10-15 parts of clay, 3-5 parts of nano-zinc oxide, 1-10 parts of colorant, 5-15 parts of potassium feldspar, 1-5 parts of spiny bean gum, 0.3-0.5 parts of sodium tripolyphosphate, and 50-60 parts of water.

[0006] Preferably, the preparation method of the modified silicon carbide fiber in step (1) is: (a) mixing N-aminoethyl-γ-aminopropyltrimethoxysilane, silicon carbide fiber, anhydrous ethanol, and deionized water, centrifuging, washing, and drying to obtain amino-modified silicon carbide fiber; (b) adding 2,6-dialdehyde-1,5-dihydroxynaphthalene, dioxane, and acetic acid to the amino-modified silicon carbide fiber for reaction, and then centrifuging, washing, and drying to obtain the functionalized silicon carbide fiber; (c) Adding MgCl2 solution to the functionalized silicon carbide fiber and adding ammonia water dropwise to react, followed by centrifugation, washing, and drying to obtain the functionalized silicon carbide fiber.

[0007] Preferably, in step (a), the mass ratio of N-aminoethyl-γ-aminopropyltrimethoxysilane, silicon carbide fiber, anhydrous ethanol, and deionized water is (1-5): (10-15): (70-90): (10-30); the reaction temperature is 25-30° C., and the reaction time is 10-12 h.

[0008] Preferably, in step (b), the usage ratio of amino-modified silicon carbide fiber, 2,6-dialdehyde-1,5-dihydroxynaphthalene, dioxane, and acetic acid is 20-50 mg:10-30 mg:1-2 mL:0.5-1 mL; the concentration of acetic acid is 4-8 mol / L; the reaction temperature is 110-130° C., and the reaction time is 72-84 h.

[0009] Preferably, in step (c), the mass concentration of the MgCl2 solution is 1-3%; the usage ratio of the functionalized silicon carbide fiber, the MgCl2 solution, and the ammonia water is 1 g: 20-30 mL: 3-5 mL; the reaction temperature is 30-40°C, and the reaction time is 2-3 h.

[0010] Preferably, in step (1), the mass ratio of the total mass of the green body raw material, water, and water reducer is 1: (0.4-0.5): (0.04-0.05); the mesh size of the sieve is 150-200; the water reducer is sodium silicate; the ball milling time is 7-8h; the inlet air temperature of the spray drying is 180-200°C; the outlet air temperature is 100-120°C; and the chemical composition of the mine waste is SiO2≥55 wt%, Al2O3≥15 wt%.

[0011] Preferably, in step (2), the temperature for drying the green body is 200-250°C, and the time for drying the green body is 45-50 minutes.

[0012] Preferably, in step (3), the temperature for drying the green tiles is 100-150°C, and the drying time is 24-36 hours; the temperature for sintering the glazed green tiles is 1100-1200°C, and the sintering time is 1-2 hours; and the colorant is any one of iron oxide yellow, chrome tin red, plum green, and malachite green.

[0013] Compared with the prior art, the beneficial effects of the present invention are mainly: (1) The present invention significantly improves the strength and thermal stability of the fiber surface by adding modified silicon carbide fiber to the raw material of the green body. Through an innovative modification process, the silicon carbide fiber is first surface treated with N-aminoethyl-γ-aminopropyltrimethoxysilane and 2,6-dialdehyde-1,5-dihydroxynaphthalene. Through the Schiff base reaction between the amino group and the aldehyde group of the silane coupling agent, a covalent organic framework structure containing a rigid naphthalene ring is established on the fiber surface, thereby improving the interfacial bonding strength and mechanical properties of the fiber. Subsequently, magnesium hydroxide is deposited on the fiber surface to form a flower-like magnesium hydroxide-coated fiber structure, further enhancing the strength and thermal stability of the fiber surface. The modified fiber has better dispersion in the sintered tile green body.

[0014] (2) The present invention significantly improves the performance of sintered tile glazes by introducing spiny bean gum into them. Spiny bean gum can form a dense network structure in the glaze. On the one hand, it fills the gaps between glaze particles, reduces the penetration channels of water, and effectively reduces the water absorption rate of the glaze. On the other hand, this structure can restrict the free movement of water, reduce the crystallization and expansion of water at low temperatures, and thus significantly improve the frost resistance of the glaze.

[0015] (3) The high-strength sintered tiles obtained by the preparation method of the high-strength sintered tiles of the present invention have the advantages of low water absorption, high bending strength, good frost resistance, high thermal stability, etc., and have broad application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 This is a scanning electron microscope image of the modified silicon carbide fiber prepared in Example 1 of the present invention. DETAILED DESCRIPTION

[0017] The technical solution of the present invention will be further described below in conjunction with specific embodiments. However, it should be understood by those skilled in the art that the following examples are only intended to illustrate the present invention and should not be construed as limiting the present invention. Specific conditions not specified in the examples are to be followed according to conventional conditions or the conditions recommended by the manufacturer. All reagents or instruments used, unless otherwise specified, are conventional products obtained from commercial channels.

[0018] Example 1 A method for preparing a high-strength sintered tile comprises the following steps: (1) N-aminoethyl-γ-aminopropyltrimethoxysilane, silicon carbide fiber (diameter 5-15 μm), anhydrous ethanol, and deionized water were mixed in a mass ratio of 3:12:80:20, reacted at 27°C for 11 hours, centrifuged, washed, and dried to obtain amino-modified silicon carbide fiber; amino-modified silicon carbide fiber, 2,6-dialdehyde-1,5-dihydroxynaphthalene, dioxane, and 6 mol / L acetic acid were mixed in a mass ratio of 35 mg:20 mg:1 mL:0.7 mL, reacted at 120°C for 78 hours; after the reaction, centrifuged, washed, and dried to obtain functionalized silicon carbide fiber; functionalized silicon carbide fiber, 2% MgCl2 solution, and 25 wt% ammonia water were mixed in a mass ratio of 1 g:25 mL:4 mL, reacted at 35°C for 2 hours; after the reaction, centrifuged, washed, and dried to obtain modified silicon carbide fiber. Scanning electron microscopy was used to characterize the microstructure of the modified silicon carbide fibers. Figure 1 shown.

[0019] (2) Ball milling and pulverizing: The green body raw material is crushed and passed through a 170 mesh sieve, and then water and sodium silicate are added and ball milled for 7 hours. After ball milling, the green body raw material is spray dried. The inlet air temperature of the spray drying is 190°C and the outlet air temperature is 110°C. The powder is obtained. The mass ratio of the total mass of the green body raw material, water, and sodium silicate is 1:0.4:0.04. The green body raw material includes the following components in parts by mass: 55 parts of mine waste, 15 parts of bentonite, 17 parts of clay, 15 parts of potassium feldspar, 7 parts of quartz, and 7 parts of modified silicon carbide fiber. The chemical composition of the mine waste is SiO2 ≥ 55 wt % and Al2O3 ≥ 15 wt %.

[0020] (3) Molding and drying: The powder obtained in step (2) is pressed into a green body; the green body is dried at 220°C for 47 minutes to obtain a green tile; (4) Glazing and firing: applying a glaze to the green tile obtained in step (3), and drying at 125°C for 30 hours to obtain a glazed green tile; sintering the glazed green tile at 1150°C for 1 hour, and then cooling to room temperature to obtain a green tile; the glaze comprises the following components in parts by mass: 35 parts of nano-silica, 12 parts of clay, 4 parts of nano-zinc oxide, 6 parts of yellow iron oxide, 10 parts of potassium feldspar, 3 parts of spiny bean gum, 0.4 parts of sodium tripolyphosphate, and 55 parts of water.

[0021] This embodiment also provides a high-strength sintered tile obtained by the above-mentioned preparation method.

[0022] Example 2 A method for preparing a high-strength sintered tile comprises the following steps: (1) N-aminoethyl-γ-aminopropyltrimethoxysilane, silicon carbide fiber, anhydrous ethanol and deionized water were mixed in a mass ratio of 1:10:70:10, reacted at 25°C for 10 h, centrifuged, washed and dried to obtain amino-modified silicon carbide fiber; amino-modified silicon carbide fiber, 2,6-dialdehyde-1,5-dihydroxynaphthalene, dioxane and 4 mol / L acetic acid were mixed in a mass ratio of 20 mg:10 mg:1 mL:0.5 mL, reacted at 110°C for 72 h; after the reaction, centrifuged, washed and dried to obtain functionalized silicon carbide fiber; functionalized silicon carbide fiber, 1% MgCl2 solution and 25 wt% ammonia water were mixed in a mass ratio of 1 g:20 mL:3 mL, reacted at 30°C for 2 h; after the reaction, centrifuged, washed and dried to obtain modified silicon carbide fiber.

[0023] (2) Ball milling and powdering: The green body raw materials were crushed and passed through a 150-mesh sieve, and then water and sodium silicate were added and ball milled for 7 hours. After ball milling, the green body raw materials were spray-dried. The inlet air temperature of the spray drying was 180°C and the outlet air temperature was 100°C. The powder was obtained. The mass ratio of the total mass of the green body raw materials, water, and sodium silicate was 1:0.4:0.04. The green body raw materials included the following components in parts by mass: 50 parts of mine waste, 10 parts of bentonite, 15 parts of clay, 10 parts of potassium feldspar, 5 parts of quartz, and 5 parts of modified silicon carbide fiber. The chemical composition of the mine waste was SiO2 ≥ 55 wt % and Al2O3 ≥ 15 wt %.

[0024] (3) Molding and drying: the powder obtained in step (2) is pressed into a green body; the green body is dried at 200°C for 45 minutes to obtain a green tile; (4) Glazing and firing: applying a glaze to the green tile obtained in step (3), and drying at 100°C for 24 hours to obtain a glazed green tile; sintering the glazed green tile at 1100°C for 1 hour, and then cooling to room temperature to obtain a green tile; the glaze comprises the following components in parts by mass: 30 parts of nano-silicon dioxide, 10 parts of clay, 3 parts of nano-zinc oxide, 1 part of yellow iron oxide, 5 parts of potassium feldspar, 5 parts of spiny bean gum, 0.3 parts of sodium tripolyphosphate, and 50 parts of water.

[0025] This embodiment also provides a high-strength sintered tile obtained by the above-mentioned preparation method.

[0026] Example 3 A method for preparing a high-strength sintered tile comprises the following steps: (1) N-aminoethyl-γ-aminopropyltrimethoxysilane, silicon carbide fiber, anhydrous ethanol and deionized water were mixed in a mass ratio of 5:15:90:30, reacted at 30℃ for 12h, centrifuged, washed and dried to obtain amino-modified silicon carbide fiber; amino-modified silicon carbide fiber, 2,6-dialdehyde-1,5-dihydroxynaphthalene, dioxane and 8mol / L acetic acid were mixed in a mass ratio of 50mg:30mg:2mL:1mL, reacted at 130℃ for 84h; after reaction, centrifuged, washed and dried to obtain functionalized silicon carbide fiber; functionalized silicon carbide fiber, MgCl2 solution with a mass concentration of 3% and ammonia water with a mass concentration of 25 wt% were mixed in a mass ratio of 1g:30mL:5mL, reacted at 40℃ for 3h; after reaction, centrifuged, washed and dried to obtain modified silicon carbide fiber.

[0027] (2) Ball milling and pulverizing: The green body raw materials are crushed and passed through a 200-mesh sieve, and then water and sodium silicate are added and ball milled for 7-8 hours. After ball milling, the green body raw materials are spray dried. The air inlet temperature of the spray drying is 200°C and the air outlet temperature is 120°C. The powder is obtained. The mass ratio of the total mass of the green body raw materials, water, and sodium silicate is 1:0.5:0.05. The green body raw materials include the following components in parts by mass: 60 parts of mine waste, 20 parts of bentonite, 20 parts of clay, 20 parts of potassium feldspar, 10 parts of quartz, and 10 parts of modified silicon carbide fiber. The chemical composition of the mine waste is SiO2 ≥ 55 wt % and Al2O3 ≥ 15 wt %.

[0028] (3) Molding and drying: the powder obtained in step (2) is pressed into a green body; the green body is dried at 250°C for 50 minutes to obtain a green tile; (4) Glazing and firing: applying the glaze to the green tile obtained in step (3), and drying at 150°C for 36 hours to obtain a glazed green tile; sintering the glazed green tile at 1200°C for 2 hours, and then cooling to room temperature to obtain a green tile; the glaze raw materials include the following components in parts by mass: 40 parts of nano-silica, 15 parts of clay, 5 parts of nano-zinc oxide, 10 parts of yellow iron oxide, 15 parts of potassium feldspar, 5 parts of spiny bean gum, 0.5 parts of sodium tripolyphosphate, and 60 parts of water.

[0029] This embodiment also provides a high-strength sintered tile obtained by the above-mentioned preparation method.

[0030] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that the modified silicon carbide fiber in the blank raw material of step (2) is replaced by silicon carbide fiber.

[0031] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that the modified silicon carbide fiber in the blank raw material of step (2) is replaced by the functionalized silicon carbide fiber of step (1).

[0032] Comparative Example 3 The difference between Comparative Example 3 and Example 1 is that the spiny bean gum in the glaze raw materials of step (4) is omitted.

[0033] Test Example 1 According to GB / T 36584-2018 "Test Methods for Roof Tiles", the water absorption, bending resistance, frost resistance, and rapid cooling and heating resistance of the high-strength sintered tiles obtained in Examples 1-3 and Comparative Examples 1-3 were measured. The results are shown in Table 1.

[0034] Table 1 Physical index test results of high-strength sintered tiles The results are shown in Table 1, which are the physical index test results of the high-strength sintered tiles prepared by Examples 1-3 of the present invention and Comparative Examples 1-3. As can be seen from Table 1, compared with Comparative Examples 1 and 2, by adding modified silicon carbide fibers to the blank raw materials, the flexural strength and thermal stability of the fiber surface can be significantly improved. The high-strength sintered tiles prepared by Examples 1-3 of the present invention have high flexural strength and good resistance to rapid cooling and heating; compared with Comparative Example 3, by introducing prickly bean gum into the sintered tile glaze, the water absorption rate of the glaze can be reduced and the frost resistance of the glaze can be improved. The high-strength sintered tiles prepared by Examples 1-3 of the present invention have low water absorption and good frost resistance. It shows that the high-strength sintered tiles obtained by the preparation method of the high-strength sintered tiles of the present invention have the advantages of low water absorption, high flexural strength, good frost resistance, high thermal stability, etc., and have broad application prospects.

[0035] Finally, it should be noted that the above embodiments are intended only to illustrate the technical solutions of the present invention and are not intended to limit the same. The basic principles and main features of the present invention have been described above using specific implementation schemes. Modifications or substitutions may be made based on the present invention, but such modifications or substitutions do not detract from the essence of the corresponding technical solutions from the scope of protection claimed by the present invention.

Claims

1. A method for preparing high-strength sintered tiles, characterized in that: The following steps are involved: (1) Ball milling and powder making: the green body raw materials are crushed and sieved, and then water and a water reducer are added for ball milling, and then spray dried after ball milling to obtain a powder; the green body raw materials include the following components by weight: 50-60 parts of mine waste, 10-20 parts of bentonite, 15-20 parts of clay, 10-20 parts of potassium feldspar, 5-10 parts of quartz, and 5-10 parts of modified silicon carbide fiber; (2) Molding and drying: the powder obtained in step (1) is pressed into a green body; the green body is dried to obtain a green tile; (3) glazing and firing: applying a glaze to the green tile obtained in step (2), and drying the green tile to obtain a glazed green tile; sintering the glazed green tile, and then cooling it to room temperature to obtain a green tile; the glaze comprises the following components in parts by weight: 30-40 parts of nano-silicon dioxide, 10-15 parts of clay, 3-5 parts of nano-zinc oxide, 1-10 parts of colorant, 5-15 parts of potassium feldspar, 1-5 parts of spiny bean gum, 0.3-0.5 parts of sodium tripolyphosphate, and 50-60 parts of water; The preparation method of the modified silicon carbide fiber in step (1) is: (a) mixing N-aminoethyl-γ-aminopropyltrimethoxysilane, silicon carbide fiber, anhydrous ethanol, and deionized water, centrifuging, washing, and drying to obtain amino-modified silicon carbide fiber; (b) adding 2,6-dialdehyde-1,5-dihydroxynaphthalene, dioxane, and acetic acid to the amino-modified silicon carbide fiber for reaction, and then centrifuging, washing, and drying to obtain the functionalized silicon carbide fiber; (c) Adding MgCl2 solution to the functionalized silicon carbide fiber and adding ammonia water dropwise to react, followed by centrifugation, washing, and drying to obtain the functionalized silicon carbide fiber.

2. The method for preparing a high-strength sintered tile according to claim 1, characterized in that: In the step (a), the mass ratio of N-aminoethyl-γ-aminopropyltrimethoxysilane, silicon carbide fiber, anhydrous ethanol, and deionized water is (1-5): (10-15): (70-90): (10-30); the reaction temperature is 25-30° C., and the reaction time is 10-12 h.

3. The method for preparing a high-strength sintered tile according to claim 1, characterized in that: In the step (b), the usage ratio of the amino-modified silicon carbide fiber, 2,6-dialdehyde-1,5-dihydroxynaphthalene, dioxane, and acetic acid is 20-50 mg: 10-30 mg: 1-2 mL: 0.5-1 mL; the concentration of acetic acid is 4-8 mol / L; the reaction temperature is 110-130° C., and the reaction time is 72-84 h.

4. The method for preparing a high-strength sintered tile according to claim 1, characterized in that: In the step (c), the mass concentration of the MgCl2 solution is 1-3%; the usage ratio of the functionalized silicon carbide fiber, the MgCl2 solution, and the ammonia water is 1 g: 20-30 mL: 3-5 mL; the reaction temperature is 30-40° C., and the reaction time is 2-3 h.

5. The method for preparing a high-strength sintered tile according to claim 1, characterized in that: In the step (1), the mass ratio of the total mass of the green body raw materials, water, and the water reducer is 1: (0.4-0.5): (0.04-0.05); the mesh size of the sieve is 150-200; the water reducer is sodium silicate; the ball milling time is 7-8 hours; the air inlet temperature of the spray drying is 180-200°C; the air outlet temperature is 100-120°C; and the chemical composition of the mine waste is SiO2≥55 wt%, Al2O3≥15 wt%.

6. The method for preparing a high-strength sintered tile according to claim 1, characterized in that: In the step (2), the temperature for drying the green body is 200-250°C, and the time for drying the green body is 45-50 minutes.

7. The method for preparing a high-strength sintered tile according to claim 1, characterized in that: In the step (3), the temperature for drying the green tiles is 100-150°C, and the drying time is 24-36 hours; the temperature for sintering the glazed green tiles is 1100-1200°C, and the sintering time is 1-2 hours; the colorant is any one of iron oxide yellow, chrome tin red, plum green, and malachite green.

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