CN110981415A - Preparation method of high-strength high-alumina ceramic sheet - Google Patents
Preparation method of high-strength high-alumina ceramic sheet Download PDFInfo
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Abstract
The invention relates to a preparation method of a high-strength high-alumina ceramic sheet, which comprises the following steps: 1) raw material treatment: respectively ball-milling coal series kaolin, calcined bauxite, common kaolin, potassium feldspar, albite and talc by using a ball mill, and sieving for later use; 2) proportioning and mixing the raw materials: weighing the raw materials according to the mass percentage, adding a green body reinforcing agent, and mixing to obtain a mixture; 3) granulating and staling; 4) semi-dry pressing and forming; 5) drying; 6) glazing; 7) and (3) firing: and (4) placing the dried blank into a roller kiln to be fired to obtain the high-strength high-alumina ceramic sheet. The method replaces industrial alumina by calcined bauxiteIntroduction of Al2O3And the strength of the ceramic sheet is enhanced by introducing the short rod-shaped mullite which is enriched and grown into the coal-series kaolin, and meanwhile, the impurity TiO of the calcined bauxite is utilized2And externally added TiO2The firing temperature is reduced, so that the prepared high-strength high-alumina ceramic sheet has the characteristics of high strength and low firing temperature, and the cost is saved.
Description
Technical Field
The invention relates to the technical field of building ceramics, in particular to a preparation method of a high-strength high-alumina ceramic sheet.
Background
The ceramic thin plate is an energy-saving and environment-friendly green building material, and GB/723266-Bufonis ceramic plate is specified to be a ceramic plate with a thickness of not more than 6m and an upper surface area of not more than 1.62m2The large specification of the thin brick of (2) is required to have a large breaking strength. The invention patent of China (CN201110039459.9) discloses a method for manufacturing a large silicon oxide ceramic sheet, which adopts needle-shaped wollastonite as a main raw material to prepare the large high-silicon ceramic sheet, wherein the breaking strength is 45-50 MPa. While the chemical composition of the high-alumina reinforced porcelain A12O3The content is high, so that a large amount of corundum crystal phase with high elastic modulus is generated in the ceramic blank, the blank is endowed with high strength, and the firing temperature is also increased. For example, in "development of medium-temperature high-alumina reinforced porcelain" (Foshan ceramics, 2007, 17 (6): 5-7.), A1 is prepared from kaolin and industrial alumina2O3The fracture strength of the reinforced porcelain with the content of 30.26 percent reaches 97MPa, but the minimum firing temperature still needs to reach 1250 ℃ after the sintering aid is added, and in addition, the industrial A1 is introduced2O3The use of aluminum as a source also increases the cost. Therefore, how to increase A12O3The key for preparing the enhanced high-strength high-alumina ceramic sheet is that the content can be reduced, the sintering temperature can be reduced, and the cost can be saved.
Disclosure of Invention
The invention aims to prepare a high-strength high-alumina ceramic sheet which requires A1 introduced by calcining bauxite and coal-series kaolin2O3The use of impurity A1 of calcined bauxite wood body while achieving reinforcement and cost reduction2O3The sintering temperature is reduced.
The technical scheme of the invention is as follows: a preparation method of a high-strength high-alumina ceramic sheet comprises the following steps:
1) raw material treatment: respectively ball-milling coal series kaolin, calcined bauxite, common kaolin, potassium feldspar, albite and talc for 16-20 h by using a ball mill, and sieving to prepare powder for later use.
2) Proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: 10-30% of coal series kaolin, 10-25% of calcined bauxite, 20-30% of common kaolin, 15-25% of feldspar, 0-5% of talc and 15-25% of quartz, weighing the raw materials, adding a blank reinforcing agent accounting for 0.1-0.25% of the total mass of the blank, and performing ball milling and uniform mixing to obtain a mixture;
3) granulation and staling: adding 7-10% of water by a spray drying method, granulating, and ageing for 24-36 h;
4) semi-dry pressing and forming: pressing and forming the aged blank by using a 1-3 ten thousand tons of pressing machine to obtain a ceramic sheet blank;
5) and (3) drying: drying the formed green body in a drying oven at 95-100 ℃ for 2-5 h;
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;
7) and (3) firing: and (3) placing the dried blank into a roller kiln to be fired for 3-6 h, and cooling to obtain the high-strength high-alumina ceramic sheet.
As a further setting of the invention, in the step 1), the granularity of the calcined bauxite is required to be 300-325 meshes, and other raw materials are sieved by 250 meshes;
as a further arrangement of the invention, in the step 2), the feldspar is formed by mixing potassium feldspar and albite, and the chemical composition of the mixed feldspar is required to be K2O/Na2O=2:1;
As a further configuration of the invention, in step 2), TiO in the mixed blank2The mass fraction of (A) is more than 1.2%, so that TiO can be embodied2Thereby reducing the firing temperature;
as a further setting of the invention, in the step 7), the sintering temperature range is 1180-1280 ℃.
The invention has the beneficial effects that:
1. high strength and low sintering temperature. The invention uses coal series kaolinIntroduction of a large amount of A12O3And corundum and mullite crystal phases directly introduced into the calcined bauxite improve the breaking strength of the ceramic sheet to 80-105 MPa, widen the sintering temperature range to 100 ℃, and simultaneously utilize TiO impurities of the calcined bauxite2The firing temperature is reduced to 1180 ℃ to achieve the purpose of reducing the firing temperature of the enhanced high-strength high-alumina ceramic sheet.
2. The cost is low. The invention adopts calcined bauxite and coal series kaolin to replace industrial alumina as an aluminum source, saves the raw material cost of nearly 1/2, and simultaneously consumes a large amount of solid waste coal gangue.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the specific embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Raw material treatment: respectively ball-milling coal series kaolin, calcined bauxite, common Henan kaolin, potash feldspar, albite and talc for 16h by using a ball mill, and sieving by using a 250-mesh sieve to obtain common kaolin powder, coal series kaolin powder, calcined bauxite powder, potassium feldspar powder, sodium feldspar powder and talcum powder for later use. The calcined bauxite is sieved by a 300-mesh sieve at the calcining temperature of 1500 ℃. The chemical compositions of the calcined alumite and the coal-series kaolin are shown in the following table:
composition (I) | SiO2 | Al2O3 | Fe2O3 | TiO2 | CaO | MgO | K2O | Na2O | I/L | Total up to |
Calcined bauxite | 7.68 | 85.11 | 0.85 | 4.22 | 0.32 | 0.24 | 0.69 | 0.07 | 0.38 | 99.5 |
Coal series kaolin | 48.9 | 35.46 | 0.12 | 0.4 | 0.038 | 0 | 0.03 | 0 | 14.7 | 99.75 |
2) Proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: weighing 10% of coal-series kaolin, 10% of calcined bauxite, 20% of common kaolin, 15% of feldspar (potassium feldspar 10%, albite 5%) and 15% of quartz, adding a blank reinforcing agent accounting for 0.1% of the total mass of the blank, uniformly mixing by using a ball mill to obtain a mixture, and adding powdery TiO2Until TiO in the mixture2The content is 1.23%:
3) granulation and staling: adding 7% of water, granulating, and aging for 24 h.
4) Semi-dry pressing and forming: placing the aged blank in a mold, compacting under 40MPa, and maintaining the pressure for 10 s;
5) and (3) drying: drying the formed green body at 95 ℃ for 2 h;
6) glazing: applying a layer of thin glaze on the green body, and drying at 80 ℃ for 30 min;
7) and (3) firing: and (3) placing the dried blank into a roller kiln to be fired at 1180 ℃ to obtain the high-strength high-alumina ceramic sheet.
The test shows that the high-strength high-alumina ceramic sheet has the thickness of 5mm, the green strength of 5.04MPa, the water absorption of 0.41 percent, the apparent porosity of 1.46 percent, the breaking strength of 90MPa, flat appearance without warping, the firing shrinkage of 9.56 percent and the volume density of 2.34g.cm-2All meet the requirements of GB/723266-2009 ceramic plate.
Example 2
Raw material treatment: respectively ball-milling coal series kaolin, calcined bauxite, common Henan kaolin, potash feldspar, albite and talc for 20h by using a ball mill, and sieving by using a 250-mesh sieve to obtain common kaolin powder, coal series kaolin powder, calcined bauxite powder, potassium feldspar powder, sodium feldspar powder and talcum powder for later use. The calcined bauxite is sieved by a 325-mesh sieve with the specification, and the calcining temperature is 1500 ℃. The chemical compositions of the calcined alumite and the coal-series kaolin are shown in the following table:
composition (I) | SiO2 | Al2O3 | Fe2O3 | TiO2 | CaO | MgO | K2O | Na2O | I/L | Total up to |
Calcined bauxite | 7.68 | 85.11 | 0.85 | 4.22 | 0.32 | 0.24 | 0.69 | 0.07 | 0.38 | 99.5 |
Coal series kaolin | 48.9 | 35.46 | 0.12 | 0.4 | 0.038 | 0 | 0.03 | 0 | 14.7 | 99.75 |
2) Proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: 30 percent of coal-series kaolin, 25 percent of calcined bauxite, 30 percent of common kaolin, 25 percent of feldspar (16.67 percent of potassium feldspar, 8.33 percent of albite), 5 percent of talcum and 25 percent of quartz, weighing the raw materials, adding a green body reinforcing agent accounting for 0.25 percent of the total mass of the blank, uniformly mixing the raw materials in a ball mill to obtain a mixture, and adding powdery TiO2Until TiO in the mixture2The content is 1.29%:
3) granulation and staling: adding 10% water, granulating, and aging for 36 hr.
4) Semi-dry pressing and forming: placing the aged blank in a mold, compacting under 40MPa, and maintaining the pressure for 10 s;
5) and (3) drying: drying the molded green body at 100 ℃ for 5 hours;
6) glazing: applying a layer of thin glaze on the green body, and drying for 1h at 100 ℃;
7) and (3) firing: and (3) putting the dried blank into a roller kiln, and firing at 1280 ℃ to obtain the high-strength high-alumina ceramic sheet.
The test shows that the high-strength high-alumina ceramic sheet has the thickness of 5mm, the green strength of 5.95MPa and the water absorption0.53%, apparent porosity of 1.25%, breaking strength of 115MPa, smooth appearance without warpage, firing shrinkage of 8.65%, and bulk density of 2.95g.cm-2All meet the requirements of GB/723266-2009 ceramic plate.
Example 3
Raw material treatment: respectively ball-milling coal series kaolin, calcined bauxite, common Henan kaolin, potash feldspar, albite and talc for 18h by using a ball mill, and sieving by using a 250-mesh sieve to obtain common kaolin powder, coal series kaolin powder, calcined bauxite powder, potassium feldspar powder, sodium feldspar powder and talcum powder for later use. The calcined bauxite is sieved by a 310-mesh sieve at the calcining temperature of 1500 ℃. The chemical compositions of the calcined alumite and the coal-series kaolin are shown in the following table:
composition (I) | SiO2 | Al2O3 | Fe2O3 | TiO2 | CaO | MgO | K2O | Na2O | I/L | Total up to |
Calcined bauxite | 7.68 | 85.11 | 0.85 | 4.22 | 0.32 | 0.24 | 0.69 | 0.07 | 0.38 | 99.5 |
Coal series kaolin | 48.9 | 35.46 | 0.12 | 0.4 | 0.038 | 0 | 0.03 | 0 | 14.7 | 99.75 |
2) Proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: the coal-series kaolin is prepared by weighing 16.67% of coal-series kaolin, 13.89% of calcined bauxite, 24.74% of common kaolin, 21.60% of feldspar (14.4% of potassium feldspar, 7.2% of albite), 2.82% of talc and 20.29% of quartz, adding 0.2% of TY-2 blank reinforcing agent, uniformly mixing by a ball mill to obtain a mixture, and adding powdery TiO2Until TiO in the mixture2The content is 1.27%:
3) granulation and staling: adding 9% water, granulating, and aging for 30 hr.
4) Semi-dry pressing and forming: placing the aged blank in a mold, compacting under 40MPa, and maintaining the pressure for 10 s;
5) and (3) drying: drying the formed green body at 98 ℃ for 3 h;
6) glazing: applying a layer of thin glaze on the green body, and drying at 90 ℃ for 45 min;
7) and (3) firing: and (4) placing the dried blank into a roller kiln to be sintered at 1200 ℃ to obtain the high-strength high-alumina ceramic sheet.
Through tests, the high-strength high-alumina ceramic sheet has the thickness of 5mm, the green strength of 5.12MPa, the water absorption of 0.49 percent, the apparent porosity of 1.30 percent, the breaking strength of 97MPa, smooth and warp-free appearance, the firing shrinkage of 9.01 percent and the volume density of 2.58g.cm < -2 >, and all meet the requirements of GB/723266 ceramic plate 2009.
Comparative example 1
Raw material treatment: respectively ball-milling the Longyan kaolin mud, the industrial alumina, the common Henan kaolin, the potash feldspar, the albite and the talc for 18h by using a ball mill, and sieving by using a 250-mesh sieve to obtain common kaolin powder, coal-series kaolin powder, calcined bauxite powder, potassium feldspar powder, sodium feldspar powder and talcum powder for later use. The calcined bauxite is sieved by a 310-mesh sieve at the calcining temperature of 1500 ℃. The chemical compositions of the calcined alumite and the coal-series kaolin are shown in the following table:
2) proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: 16.67 percent of Longyan kaolin mud washing, 13.89 percent of industrial alumina, 24.74 percent of common kaolin, 21.60 percent of feldspar (14.4 percent of potassium feldspar, 7.2 percent of albite), 2.82 percent of talcum and 20.29 percent of quartz are weighed, 0.2 percent of TY-2 blank reinforcing agent is added into the raw materials, the raw materials are uniformly mixed by a ball mill to obtain a mixture, and TiO in the mixture is uniformly mixed to obtain a mixture2Content (wt.)About 0.09%.
3) Granulation and staling: adding 9% water, granulating, and aging for 30 hr.
4) Semi-dry pressing and forming: placing the aged blank in a mold, compacting under 40MPa, and maintaining the pressure for 10 s;
5) and (3) drying: drying the formed green body at 98 ℃ for 3 h;
6) glazing: applying a layer of thin glaze on the green body, and drying at 90 ℃ for 45 min;
7) and (3) firing: and putting the dried blank into a roller kiln, and firing at 1260 ℃ to obtain the high-strength high-alumina ceramic sheet.
The test shows that the high-strength high-alumina ceramic sheet has the thickness of 5mm, the green strength of 4.03MPa, the water absorption of 0.76%, the apparent porosity of 1.92%, the breaking strength of 72MPa, smooth appearance, no warpage, the sintering shrinkage of 10.31%, and the volume density of 2.06g.cm-2All meet the requirements of GB/723266-2009 ceramic plate.
Comparative example 2
Raw material treatment: respectively ball-milling the Longyan kaolin mud, the industrial alumina, the common Henan kaolin, the potash feldspar, the albite and the talc for 18h by using a ball mill, and sieving by using a 250-mesh sieve to obtain common kaolin powder, coal-series kaolin powder, calcined bauxite powder, potassium feldspar powder, sodium feldspar powder and talcum powder for later use. The calcined bauxite is sieved by a 310-mesh sieve at the calcining temperature of 1500 ℃. The chemical compositions of the calcined alumite and the coal-series kaolin are shown in the following table:
2) proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: 16.67 percent of Longyan kaolin mud washing, 13.89 percent of industrial alumina, 24.74 percent of common kaolin, 21.60 percent of feldspar (10.8 percent of potassium feldspar, 10.8 percent of albite), 2.82 percent of talcum and 20.29 percent of quartz are weighed, 0.2 percent of TY-2 blank reinforcing agent is added into the raw materials, the raw materials are uniformly mixed by a ball mill to obtain a mixture, and TiO in the mixture is uniformly mixed to obtain a mixture2The content is about 0.09%.
3) Granulation and staling: adding 9% water, granulating, and aging for 30 hr.
4) Semi-dry pressing and forming: placing the aged blank in a mold, compacting under 40MPa, and maintaining the pressure for 10 s;
5) and (3) drying: drying the formed green body at 98 ℃ for 3 h;
6) glazing: applying a layer of thin glaze on the green body, and drying at 90 ℃ for 45 min;
7) and (3) firing: and putting the dried blank into a roller kiln, and firing at 1260 ℃ to obtain the high-strength high-alumina ceramic sheet.
The test shows that the high-strength high-alumina ceramic sheet has the thickness of 5mm, the green strength of 3.83MPa, the water absorption of 0.79 percent, the apparent porosity of 1.96 percent, the breaking strength of 70MPa, smooth appearance without warping, the firing shrinkage of 10.62 percent and the volume density of 2.10g.cm-2All meet the requirements of GB/723266-2009 ceramic plate.
Claims (5)
1. The preparation method of the high-strength high-alumina ceramic sheet is characterized by comprising the following steps of:
1) raw material treatment: respectively ball-milling coal series kaolin, calcined bauxite, common kaolin, potassium feldspar, albite and talc for 16-20 hours by using a ball mill, and sieving to prepare powder for later use;
2) proportioning and mixing the raw materials: the weight percentage of each raw material is as follows: 10-30% of coal series kaolin, 10-25% of calcined bauxite, 20-30% of common kaolin, 15-25% of feldspar, 0-5% of talc and 15-25% of quartz, weighing the raw materials, adding a blank reinforcing agent accounting for 0.1-0.25% of the total mass of the blank, and performing ball milling and uniform mixing to obtain a mixture;
3) granulation and staling: adding 7-10% of water by a spray drying method, granulating, and ageing for 24-36 h;
4) semi-dry pressing and forming: pressing and forming the aged blank by using a 1-3 ten thousand tons of pressing machine to obtain a ceramic sheet blank;
5) and (3) drying: drying the formed green body in a drying oven at 95-100 ℃ for 2-5 h;
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;
7) and (3) firing: and (3) placing the dried blank into a roller kiln to be fired for 3-6 h, and cooling to obtain the high-strength high-alumina ceramic sheet.
2. The method for preparing a high-strength high-alumina ceramic sheet as claimed in claim 1, wherein: in the step 1), the granularity of the calcined bauxite is required to be 300-325 meshes, and other raw materials are sieved by 250 meshes.
3. The method for preparing a high-strength high-alumina ceramic sheet as claimed in claim 1, wherein: in the step 2), the feldspar is formed by mixing potassium feldspar and albite, and the mixed feldspar is required to be chemically composed of K2O/Na2O=2:1。
4. The method for preparing a high-strength high-alumina ceramic sheet as claimed in claim 1, wherein: in the step 2), powdery TiO is also added2Until the mixed blank contains TiO2Is greater than 1.2 percent.
5. The method for preparing a high-strength high-alumina ceramic sheet as claimed in claim 1, wherein: in the step 7), the sintering temperature range is 1180-1280 ℃.
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