CN107721380B - Preparation method of low-cost high-aluminum ceramic sheet - Google Patents
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Abstract
The invention relates to a preparation method of a low-cost high-aluminum ceramic sheet. The preparation method of the low-cost high-aluminum ceramic sheet is characterized by comprising the following steps of: 1) treating raw materials; 2) proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: 10-25% of coal series kaolin, 10-25% of calcined bauxite, 20-30% of common kaolin, 15-25% of feldspar, 0-5% of talc and 18-25% of quartz, and weighing the raw materials to obtain a blank; adding a reinforcing agent which is 0.1-0.25% of the total mass of the blank, ball-milling for 12-18 h, and uniformly mixing to obtain a mixture; wherein the feldspar is formed by mixing potassium feldspar and albite, and the mixed feldspar is chemically K2O/Na2O2: 1 (mass ratio); 3) granulating and staling; 4) semi-dry pressing and forming; 5) drying; 6) glazing; 7) and firing to obtain the low-cost high-alumina ceramic sheet. The firing temperature of the high-alumina ceramic sheet prepared by the method is only 1180 ℃, so that the cost is low and the strength is high.
Description
Technical Field
The invention relates to a preparation method of a low-cost high-aluminum ceramic sheet, which is mainly used as a building inner wall, an outer wall decorative plate and the like, and belongs to the field of building ceramics.
Background
The ceramic sheet is a novel green, energy-saving and environment-friendly building ceramic, and can be prepared according to Al in a blank body of the ceramic sheet2O3The content is divided into high-aluminum (Al)2O3Not less than 28%) and high Silicon (SiO)2≥60％，Al2O3< 28%) of two types. Compared with the high-silicon ceramic sheet, the high-aluminum ceramic sheet has the advantages of high strength, good corrosion resistance, difficult cracking and the like. However, the high-alumina ceramic sheet blank is generally added with industrial alumina, which causes high cost and limits the application of the ceramic sheet.
The Chinese invention patent 'a manufacturing method of a large silicon oxide ceramic sheet' (CN201110039459.9) prepares a high-silicon ceramic sheet, and the breaking strength is only 45-50 MPa; improving large-scale ultra-thin buildingThe research on the performance of ceramic blanks for building ceramic tiles (Zhoujia et al, ceramic school, 2006, 27(3): 243-; the Chinese invention patent (CN201610214106.0) discloses a method for preparing a ceramic sheet by utilizing coal gangue and potassium feldspar and a ceramic sheet prepared by the method, wherein the coal gangue is added to prepare the ceramic sheet, the strength reaches 70.29MPa, and the firing temperature is 1270 ℃; processing and properties of large-sized ceramic blocks (Raimondo, Dondi, et al. Boieti De La society
De Cer mica Y Vidrio,2010,49(4): 289-; the invention patent of China (CN104496438A) discloses a quartz sand tailing or silica sand tailing based high-strength ceramic plate and a preparation method thereof, wherein the ceramic plate is prepared from raw materials such as quartz sand tailings and the like, the firing temperature is 900 ℃, but the breaking strength is only 32-37 MPa. Therefore, how to prepare high-strength high-alumina ceramic sheets at a relatively low temperature, thereby significantly reducing the cost, is a difficult point in the ceramic industry.
Disclosure of Invention
The invention aims to provide a preparation method of a low-cost high-alumina ceramic sheet, which adopts low-cost calcined bauxite and coal series kaolin natural raw materials, and the firing temperature for preparing the high-alumina ceramic sheet is 1180 ℃, so that the cost is lower, and the strength is higher.
In order to achieve the purpose, the invention adopts the technical scheme that the preparation method of the low-cost high-aluminum ceramic sheet is characterized by comprising the following steps of:
1) raw material treatment: respectively ball-milling coal-series kaolin, calcined bauxite, common kaolin, feldspar, talc and quartz for 16-20 hours by using a ball mill, and sieving to prepare powder for later use, wherein the feldspar is potassium feldspar and albite;
2) proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: 10-25% of coal series kaolin, 10-25% of calcined bauxite, 20-30% of common kaolin, 15-25% of feldspar, 0-5% of talc and 18-25% of quartz, and weighing the raw materials to obtain a blank; adding a blank reinforcing agent which is 0.1-0.25% of the total mass of the blank, and carrying out ball milling for 12-18 h to obtain a mixture;
wherein the feldspar is formed by mixing potassium feldspar and albite, and the mixed feldspar is chemically K2O/Na2O2: 1 (mass ratio);
3) granulation and staling: adding water which is 7-10% of the mass of the mixture by adopting a spray granulation method, granulating, and then ageing for 24-36 hours to obtain an aged blank;
4) semi-dry pressing and forming: pressing and forming the aged blank by using an automatic hydraulic press to obtain a ceramic sheet blank;
5) and (3) drying: drying the formed ceramic sheet blank in a drying oven at 95-100 ℃ for 2-5 h to obtain a green blank;
6) glazing: applying a layer of thin glaze on the green body in a glaze pouring mode, and drying the green body in a drying oven at the temperature of 80-100 ℃ for 30 min-1 h to obtain a dried green body;
7) and (3) firing: and (3) placing the dried blank into a roller kiln to be fired for 3-6 h, wherein the minimum firing temperature is 1180 ℃, and cooling to obtain the low-cost high-aluminum ceramic sheet.
The calcined bauxite used in the step 1) is required to be sieved by 325 meshes, and the coal series kaolin, the common kaolin, the feldspar, the talc and the quartz are sieved by 250 meshes.
In step 2), TiO in the mixture2Is greater than 1.2 percent.
In the step 6), the thickness of one layer of thin glaze is 0.05-0.2 mm.
The coal-series kaolin is a coal-series kaolin raw ore provided by Shanxi gold ocean energy Co.
The calcined bauxite is Henan Xinmi calcined bauxite with the granularity of 325 meshes.
The common kaolin, the feldspar, the talc and the quartz are all provided by Xiangyang Gaoming mining industry Co.
The green body reinforcing agent is a Jingdezhen ceramics university TY-2 green body reinforcing agent.
The invention has the beneficial effects that:
1. the cost is low. The invention has low cost of raw materials, and calcined bauxite is used for replacing pure Al2O3As the aluminum source of the high-aluminum ceramic sheet blank, introducing another low-cost raw material, namely coal-series kaolin; on the other hand, by using TiO of calcined bauxite itself2The impurities reduce the firing temperature to 1180 ℃. The production cost of the high-alumina ceramic sheet is reduced by about 1/3 compared with other ceramic sheets, and the high-alumina ceramic sheet is favorable for popularization, production and sale.
2. The strength is higher. According to the invention, the calcined bauxite is adopted in the blank formula to introduce a corundum crystal phase with high elastic modulus (see point 1 in figure 3), so that the strength is improved; at the same time, the impurity TiO in the bauxite is calcined2Can be mixed with Al2O3A solid solution is formed (see point 3 in fig. 3) which helps the generation of a liquid phase during firing, thereby lowering the firing temperature to 1180 ℃. In addition, the coal-based kaolin is introduced into the blank formula to generate the enriched-growth short-rod mullite (shown in figure 4) in situ in the firing process, so that the internal stress of the blank is dispersed, the crack propagation path is prolonged, and the breaking strength of the ceramic sheet is improved to 84-92 MPa and exceeds 45MPa of the national standard. Thereby preparing the high-alumina ceramic sheet with low cost.
Drawings
FIG. 1 is a secondary electron image and an element plane distribution diagram of a cross section of a ceramic thin plate according to the present invention.
FIG. 2 is a secondary electron image of a cross section of a ceramic thin plate and an elemental analysis designated dot diagram according to the present invention.
FIG. 3 is the EDS spectra and phase composition analysis of the indicated points in FIG. 2.
FIG. 4 is a micrograph of a ceramic sheet blank according to the present invention.
Detailed Description
Example 1:
a preparation method of a low-cost high-alumina ceramic sheet comprises the following steps:
1) raw material treatment: respectively ball-milling coal series kaolin, calcined bauxite, common kaolin, feldspar (potassium feldspar and albite), talc and quartz for 16h by using a ball mill, and sieving to prepare powder for later use, wherein the calcined bauxite is required to be sieved by 325 meshes, and the coal series kaolin, the common kaolin, the feldspar, the talc and the quartz are respectively sieved by 250 meshes. The coal-series kaolin is coal-series kaolin crude ore provided by Shanxi gold ocean energy limited company, the calcined bauxite is Henan Xinmi calcined bauxite with the granularity of 325 meshes, common kaolin, feldspar, talc and quartz are provided by Xiangyang Gaoming mining industry limited company, and the green body reinforcing agent is TY-2 parison body reinforcing agent of Jingdezhen ceramic university;
2) proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: coal series kaolin 10%, calcined bauxite 10%, ordinary kaolin 30%, feldspar 25% (feldspar is made up by mixing potassium feldspar 18%, albite 7%, the feldspar chemical composition K after mixing)2O/Na2O2: 1), 0% of talcum and 25% of quartz, and weighing the raw materials to obtain a blank; adding a green body reinforcing agent accounting for 0.1 percent of the total mass of the blank, ball-milling for 12 hours, and uniformly mixing to obtain a mixture (TiO in the mixture)2Mass fraction of (b) is greater than 1.2%);
3) granulation and staling: adding water which is 7 percent of the mass of the mixture by adopting a spray granulation method, granulating and then aging for 24 hours to obtain an aged blank;
4) semi-dry pressing and forming: pressing and forming the aged blank by using an automatic hydraulic press to obtain a ceramic sheet blank;
5) and (3) drying: drying the formed ceramic sheet blank in a drying oven at 95 ℃ for 2h to obtain a green blank;
6) glazing: applying a layer of thin glaze (thickness 0.05mm) on the green body by adopting a glaze spraying mode, and drying in a drying oven at 80 ℃ for 30min to obtain a dried green body;
7) and (3) firing: and (3) placing the dried blank into a roller kiln to be sintered for 3 hours, wherein the minimum sintering temperature is 1180 ℃, and cooling to obtain the low-cost high-alumina ceramic sheet.
According to the test of the national standard GB/T3810 ceramic tile test method, the high-alumina ceramic sheet prepared by the invention has the water absorption of 0.38%, the breaking strength of 85MPa, and smooth and warp-free appearance, and all meet the requirements of GB/723266 ceramic tile 2009.
The minimum firing temperature is 1180 ℃, the thickness is only 3.5mm, and the requirements of actual production and use are met.
TABLE 1 results of elemental analysis and phase composition (wt%) of the points indicated in FIG. 2
Note: the results of the point 3 analysis indicate that Ti is present in the ceramic sheet4+Enter Al2O3，TiO2With Al2O3A solid solution is formed, which is a mechanism for lowering the firing temperature of the high-alumina ceramic sheet according to the present invention.
Example 2:
a preparation method of a low-cost high-alumina ceramic sheet comprises the following steps:
1) raw material treatment: respectively ball-milling coal series kaolin, calcined bauxite, common kaolin, feldspar (potassium feldspar and albite), talc and quartz for 18h by using a ball mill, and sieving to prepare powder for later use, wherein the calcined bauxite is required to be sieved by 325 meshes, and the coal series kaolin, the common kaolin, the feldspar, the talc and the quartz are respectively sieved by 250 meshes. The coal-series kaolin is coal-series kaolin crude ore provided by Shanxi gold ocean energy limited company, the calcined bauxite is Henan Xinmi calcined bauxite with the granularity of 325 meshes, common kaolin, feldspar, talc and quartz are provided by Xiangyang Gaoming mining industry limited company, and the green body reinforcing agent is TY-2 parison body reinforcing agent of Jingdezhen ceramic university;
2) proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: coal series kaolin 20%, calcined bauxite 17%, common kaolin 22%, feldspar 20% (the feldspar is formed by mixing potassium feldspar 15%, albite 5%, the feldspar chemical composition K after mixing2O/Na2O2: 1), 3% of talcum and 18% of quartz, and weighing the raw materials to obtain a blank; adding a blank reinforcing agent accounting for 0.2 percent of the total mass of the blank, and performing ball millingMixing for 16h to obtain mixture (TiO in the mixture)2Mass fraction of (b) is greater than 1.2%);
3) granulation and staling: adding water which is 8 percent of the mass of the mixture by adopting a spray drying method, granulating, and ageing for 30 hours to obtain an aged blank;
4) semi-dry pressing and forming: pressing and forming the aged blank by using an automatic hydraulic press to obtain a ceramic sheet blank;
5) and (3) drying: drying the formed ceramic sheet blank in a drying oven at 98 ℃ for 3h to obtain a green blank;
6) glazing: applying a layer of thin glaze (thickness of 0.1mm) on the green body by glaze spraying, and drying in a drying oven at 90 deg.C for 50min to obtain dried green body;
7) and (3) firing: and (3) placing the dried blank into a roller kiln to be sintered for 4 hours, wherein the minimum sintering temperature is 1180 ℃, and cooling to obtain the low-cost high-alumina ceramic sheet.
According to the test of the national standard GB/T3810 ceramic tile test method, the high-alumina ceramic sheet prepared by the invention has the water absorption of 0.42 percent, the breaking strength of 92MPa and smooth and warp-free appearance, and all meet the requirements of GB/723266 ceramic tile 2009. The minimum firing temperature is 1180 ℃, the thickness is only 4.2mm, and the requirements of actual production and use are met.
Example 3:
a preparation method of a low-cost high-alumina ceramic sheet comprises the following steps:
1) raw material treatment: respectively ball-milling coal series kaolin, calcined bauxite, common kaolin, feldspar (potassium feldspar and albite), talc and quartz for 20h by using a ball mill, and sieving to prepare powder for later use, wherein the calcined bauxite is required to be sieved by 325 meshes, and the coal series kaolin, the common kaolin, the feldspar and the talc are respectively sieved by 250 meshes. The coal-series kaolin is coal-series kaolin crude ore provided by Shanxi gold ocean energy limited company, the calcined bauxite is Henan Xinmi calcined bauxite with the granularity of 325 meshes, common kaolin, feldspar, talc and quartz are provided by Xiangyang Gaoming mining industry limited company, and the green body reinforcing agent is TY-2 parison body reinforcing agent of Jingdezhen ceramic university;
2) proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: coal series kaolin 25%, calcined bauxite 22%, ordinary kaolin 20%, feldspar 15% (feldspar is made up by mixing potassium feldspar 11%, albite 4%, the feldspar chemical composition K after mixing)2O/Na2O2: 1), talc 0% and quartz 18%, and weighing the raw materials to obtain a blank; adding a green body reinforcing agent accounting for 0.25 percent of the total mass of the blank, ball-milling for 18 hours, and uniformly mixing to obtain a mixture (so as to ensure that TiO is mixed with the green body reinforcing agent)2Exhibits fluxing action and requires TiO in the mixture2Mass fraction of (b) is greater than 1.2%);
3) granulation and staling: adding water with the mass of 10% of the mixture by adopting a spray drying method, granulating, and ageing for 36 hours to obtain an aged blank;
4) semi-dry pressing and forming: pressing and forming the aged blank by using an automatic hydraulic press to obtain a ceramic sheet blank;
5) and (3) drying: drying the formed ceramic sheet blank in a drying oven at 100 ℃ for 5 hours to obtain a green blank;
6) glazing: applying a layer of thin glaze (the thickness is 0.2mm) on the green body in a glaze pouring mode, and drying the green body in a drying oven at 100 ℃ for 1h to obtain a dried green body;
7) and (3) firing: and (3) placing the dried blank into a roller kiln to be sintered for 6h, wherein the minimum sintering temperature is 1180 ℃, and cooling to obtain the low-cost high-alumina ceramic sheet.
According to the test of the national standard GB/T3810 ceramic tile test method, the high-alumina ceramic sheet prepared by the invention has the water absorption rate of less than or equal to 0.5 percent, the breaking strength of 84-92 MPa, and smooth and warp-free appearance, and all meet the requirements of GB/723266 ceramic plate 2009. The minimum firing temperature is 1180 ℃, the thickness is only 3-6 mm, and the requirements of actual production and use are met.
Claims (5)
1. The preparation method of the low-cost high-aluminum ceramic sheet is characterized by comprising the following steps of:
1) raw material treatment: respectively ball-milling coal-series kaolin, calcined bauxite, common kaolin, feldspar, talc and quartz for 16-20 hours by using a ball mill, and sieving to prepare powder for later use, wherein the feldspar is potassium feldspar and albite;
the particle size of the calcined alumen is 325 meshes;
2) proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: 10-25% of coal series kaolin, 10-25% of calcined bauxite, 20-30% of common kaolin, 15-25% of feldspar, 0-5% of talc and 18-25% of quartz, and weighing the raw materials to obtain a blank; adding a blank reinforcing agent which is 0.1-0.25% of the total mass of the blank, and carrying out ball milling for 12-18 h to obtain a mixture;
wherein the feldspar is formed by mixing potassium feldspar and albite, and the mixed feldspar is chemically K2O/Na2The mass ratio of O is 2: 1;
3) granulation and staling: adding water which is 7-10% of the mass of the mixture by adopting a spray granulation method, granulating, and then ageing for 24-36 hours to obtain an aged blank;
4) semi-dry pressing and forming: pressing and forming the aged blank by using an automatic hydraulic press to obtain a ceramic sheet blank;
5) and (3) drying: drying the formed ceramic sheet blank in a drying oven at 95-100 ℃ for 2-5 h to obtain a green blank;
6) glazing: applying a layer of thin glaze on the green body in a glaze pouring mode, and drying the green body in a drying oven at the temperature of 80-100 ℃ for 30 min-1 h to obtain a dried green body;
7) and (3) firing: and (3) placing the dried blank into a roller kiln to be fired for 3-6 h, wherein the minimum firing temperature is 1180 ℃, and cooling to obtain the low-cost high-aluminum ceramic sheet.
2. The method for preparing a low-cost high-alumina ceramic sheet according to claim 1, wherein: the calcined bauxite used in the step 1) is required to be sieved by 325 meshes, and the coal series kaolin, the common kaolin, the feldspar, the talc and the quartz are sieved by 250 meshes.
3. The method for preparing a low-cost high-alumina ceramic sheet according to claim 1, wherein: in step 2), mixingMedium TiO 22Is greater than 1.2 percent.
4. The method for preparing a low-cost high-alumina ceramic sheet according to claim 1, wherein: in the step 2), the blank reinforcing agent is a Jingdezhen ceramics university TY-2 blank reinforcing agent.
5. The method for preparing a low-cost high-alumina ceramic sheet according to claim 1, wherein: in the step 6), the thickness of one layer of thin glaze is 0.05-0.2 mm.
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