Marble tile with low water absorption rate and preparation method thereof

Abstract

The invention discloses a low-water-absorption marble tile and a preparation method thereof, and belongs to the field of tiles. The preparation method comprises the following steps: adding water into nano aluminum oxide and clay and quartz in mineral aggregate, and carrying out ball milling to obtain a nano aluminum oxide suspension; adding water into other mineral aggregates in the mineral aggregates, performing ball milling, drying and crushing to obtain blank powder; and adding the nano aluminum oxide suspension into the blank powder, then adding soda-lime glass powder and a dispersing agent, stirring, carrying out compression molding, drying, and sintering to obtain the low-water-absorption marble ceramic tile. According to the invention, nano-alumina and clay and quartz in the mineral aggregate are subjected to ball milling together to obtain a nano-alumina suspension, and then the nano-alumina suspension is used for preparing the marble tile, so that the water absorption of the marble tile can be remarkably reduced.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of ceramic tiles, and particularly relates to a marble ceramic tile with low water absorption and a preparation method thereof. BACKGROUND

[0002] As an important building material, ceramic tiles are increasingly widely used in building decoration and interior decoration. In order to protect the walls and floors of buildings and increase the aesthetic degree, ceramic tiles are usually laid on the walls and floors, indoors and outdoors. In order to achieve the desired effect, in addition to ensuring the color, texture, wear resistance and strength requirements of the ceramic tiles, the water absorption of the ceramic tiles is also an important parameter. The water absorption directly affects the performance of the ceramic tiles and is an important indicator for evaluating the quality of the ceramic tiles. The water absorption has a great influence on the strength, linear expansion, frost resistance and impact resistance of the ceramic tiles. The ceramic tiles with low water absorption have good sintering degree, high strength and excellent comprehensive performance, and are high-grade ceramic tiles. According to the national standard GB / T 4100-2015, the water absorption of ceramic tiles is less than or equal to 0.5%.

[0003] At present, the mainstream technical route for reducing the water absorption of ceramic tiles mainly includes the following three types:

[0004] (1) High-activity flux enhanced sintering method

[0005] Lithium feldspar, nepheline syenite and other high-valence flux materials are used to reduce the sintering temperature (1100-1150℃) to promote the generation of liquid phase and densify the body. However, lithium feldspar and the like significantly increase the cost of raw materials (the unit price of lithium feldspar is 6-8 times that of potassium feldspar), and excessive use may cause side effects (such as nano agglomeration and lithium evaporation pollution of the kiln).

[0006] (2) Nano material modification method

[0007] Nano alumina, silicon carbide nanowires and other materials are added to refine the grain boundaries, but the dispersion of nano materials is difficult (ultrasonic treatment for more than 30 minutes is required), and the reduction of water absorption is limited. When the addition amount exceeds 3%, the bending strength decreases by 20-30%.

[0008] (3) High-pressure forming densification method

[0009] Ultra-high pressure forming (50-60MPa) is used to reduce the initial porosity of the body, but high-hardness molds (tungsten steel) are required, which increases the equipment investment cost by 50%, and the body demolding crack rate increases to 5-8%.

[0010] Therefore, it is of important application prospect to provide a low-cost method for significantly reducing the water absorption of ceramic tiles. SUMMARY

[0011] In order to overcome the deficiencies of the prior art, the present application provides a marble tile with low water absorption and a preparation method thereof; the present application improves the preparation method of the marble tile based on nano-alumina, which can significantly reduce the water absorption of the tile, has high bending strength, low alkali precipitation, and does not obviously increase the cost.

[0012] The technical scheme adopted by the present application to solve the technical problems is:

[0013] The present application provides a preparation method of a marble tile with low water absorption, comprising the following steps:

[0014] (1) ball milling nano-alumina, a dispersing agent, and clay and quartz in the mineral material together with water to obtain a nano-alumina suspension;

[0015] (2) ball milling potash feldspar, black mica, soda feldspar, glaze recovery material, body recovery material, zirconium silicate, porcelain stone, recycled plastic material, and kaolin (the rest of the mineral material) in the mineral material with water, drying, crushing, to obtain a body powder;

[0016] (3) adding the nano-alumina suspension of step (1) into the body powder of step (2), then adding sodium-calcium glass powder and a dispersing agent, stirring, pressing into shape, drying, and firing to obtain a marble tile with low water absorption;

[0017] The raw materials of the marble tile with low water absorption include mineral material, sodium-calcium glass powder, nano-alumina, and a dispersing agent;

[0018] The mineral material includes the following components by mass fraction: 6.0-10.0 parts of potash feldspar, 1.0-4.5 parts of black mica, 12-16 parts of quartz, 8-12 parts of soda feldspar, 1.0-1.5 parts of glaze recovery material, 6-12 parts of body recovery material, 10-16 parts of zirconium silicate, 4.5-6 parts of porcelain stone, 3-4 parts of recycled plastic material, 5-10 parts of kaolin, and 17-24 parts of clay;

[0019] The amount of the sodium-calcium glass powder is 0%-6% of the mass of the mineral material;

[0020] The amount of the nano-alumina is 1%-3% of the mass of the mineral material;

[0021] The amount of the dispersing agent in step (1) is 0.1%-0.5% of the mass of the nano-alumina;

[0022] The amount of the dispersing agent in step (3) is 0.05%-0.2% of the mass of the mineral material.

[0023] Preferably, the amount of the sodium-calcium glass powder is 2%-6% of the mass of the mineral material. After adding the sodium-calcium glass powder, the water absorption can be further reduced, the alkali precipitation can be reduced, and the bending strength can be improved.

[0024] Preferably, the amount of nano-alumina is 1% to 2% of the mass of the mineral aggregate.

[0025] Further preferably, the amount of sodium-calcium glass powder is 2% to 4% of the mass of the mineral aggregate.

[0026] The amount of nano-alumina is 1% to 2% of the mass of the mineral aggregate. The amount of sodium-calcium glass powder is 2% to 4% of the mass of the mineral aggregate, and the brick surface is free of carbon bubbles and impurities.

[0027] More preferably, the amount of sodium-calcium glass powder is 4% of the mass of the mineral aggregate.

[0028] The amount of nano-alumina is 2% of the mass of the mineral aggregate.

[0029] Preferably, the mineral aggregate includes the following components in parts by mass: star potassium sand 6.0 to 10.0 parts, lusitanian black mica 1.0 to 4.5 parts, jintao stone powder 12 to 16 parts, rong sodium stone powder 8 to 12 parts, glaze mud 1.0 to 1.5 parts, edge grinding mud 6 to 12 parts, mingshi powder 10 to 16 parts, rongsheng stone powder 4.5 to 6 parts, pressed mud 3 to 4 parts, foreign kaolin 5 to 10 parts, yongli mud 7 to 9 parts, huicheng mud 7 to 9 parts, and coffee mud 3 to 6 parts. Among them, yongli mud, huicheng mud, and coffee mud are clay, and jintao stone powder is quartz.

[0030] Preferably, in step (1), the particle size of the nano-alumina is 20 to 50 nm.

[0031] Preferably, in step (1), the dispersing agent is sodium polyacrylate.

[0032] Preferably, in step (1), the water ball milling time is 4 to 6 hours, and the mass ratio of the material to water for water ball milling is 1:(0.6-1.0).

[0033] Preferably, in step (2), the mass ratio of the material to water for water ball milling is (60-65):(35-40), and the time is 10 to 20 minutes.

[0034] Preferably, in step (2), the moisture content of the obtained green powder is 5% to 7.0%, and the particle size is 40 to 60 mesh.

[0035] Preferably, in step (3), the particle size of the sodium-calcium glass powder is D50=10-15 μm.

[0036] Preferably, in step (3), the components of the sodium-calcium glass powder are: SiO268-76%, Na2O 11-14%, CaO 9-11%, Fe2O3≤0.05%, MgO 0.8%-1.2%, and the balance is other components.

[0037] Preferably, in step (3), the dispersing agent is sodium polyacrylate.

[0038] Preferably, in step (3), the stirring speed is 45-60 rpm, and the stirring time is 30-60 minutes.

[0039] Preferably, in step (3), the pressure for the press forming is 3200-3500T, and the pressure holding time is 5-10 seconds.

[0040] Preferably, in step (3), the water content of the dried green body is ≤0.8%.

[0041] Preferably, in step (3), the firing parameters are as follows: the temperature is raised from room temperature to 600℃ at a rate of 20-50℃ / min, the temperature is raised from 600℃ to 1000℃ at a rate of 60-70℃ / min, the temperature is raised from 1000℃ to 1230℃ at a rate of 50-60℃ / min, the temperature is kept at 1230℃ for 15-20 minutes, the temperature is lowered from 1230℃ to 600℃ at a rate of 120-150℃ / min, and the temperature is lowered from 600℃ to room temperature at a rate of 20-30℃ / min.

[0042] Preferably, in step (3), the glaze is applied, inkjet printing is performed, and the protective glaze is applied before drying and firing.

[0043] The present application provides a marble ceramic tile with low water absorption prepared by the above preparation method.

[0044] The marble ceramic tile prepared by the present application has a water absorption of ≤0.37%, a surface efflorescence of ≤0.19mg / cm 2 , and a bending strength of ≥38.7MPa.

[0045] Preferably, the marble ceramic tile prepared by the present application has a water absorption of ≤0.05%, a surface efflorescence of ≤0.015mg / cm 2 , and a bending strength of ≥54.4MPa.

[0046] The present application has the following advantages:

[0047] The present application improves the preparation process of marble ceramic tile doped with nano-alumina, and the nano-alumina is ball milled with clay and quartz in the mineral material after adding water to obtain a nano-alumina suspension, which is then used to prepare marble ceramic tile, which can significantly reduce the water absorption of marble ceramic tile; meanwhile, the marble ceramic tile has high bending strength, and the cost does not increase significantly. DETAILED DESCRIPTION

[0048] The present application is further illustrated by the following examples.

[0049] The concept, specific scheme and generated technical effects of the present application will be described clearly and completely in combination with the embodiments below, so as to fully understand the purpose, features and effects of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, but not all the embodiments, and other embodiments obtained by those skilled in the art on the basis of the embodiments of the present application without creative labor are within the protection scope of the present application. Each technical feature in the present application can be combined with each other as long as they are not contradictory.

[0050] The present application provides a preparation method of marble ceramic tile with low water absorption, comprising the following steps:

[0051] The basic raw materials include mineral materials, sodium-calcium glass powder, nano-alumina and dispersant;

[0052] The mineral materials include the following components in mass fraction: 6.0-10.0 parts of star potassium sand, 1.0-4.5 parts of lusong black mica, 12-16 parts of jintao stone powder, 8-12 parts of rong sodium stone powder, 1.0-1.5 parts of glaze mud, 6-12 parts of edge grinding mud, 10-16 parts of mingshi powder, 4.5-6 parts of rongsheng stone powder, 3-4 parts of squeezing mud, 5-10 parts of foreign kaolin, 7-9 parts of yongli mud, 7-9 parts of huicheng mud, and 3-6 parts of coffee mud;

[0053] The amount of the sodium-calcium glass powder is 0%-6% of the mass of the mineral materials;

[0054] The amount of the nano-alumina is 1%-3% of the mass of the mineral materials;

[0055] (1) Pretreatment of raw materials

[0056] (1.1) Preparation of sodium-calcium glass powder

[0057] Sorting and impurity removal:

[0058] After crushing, the sodium-calcium glass is removed by a color sorter (wavelength 500-600 nm) to remove colored impurities (such as green beer bottle glass), so as to ensure that the whiteness of the glass powder is >80%.

[0059] Magnetic separation for removing iron:

[0060] A high gradient magnetic separator (magnetic field strength 1.2T) is used to remove metal impurities, and the content of Fe2O3 is controlled to be ≤0.1%.

[0061] Ultrafine grinding:

[0062] The glass powder is ground through a 300-330 mesh screen by using an air jet mill, D50=10-15μm, and the particle size distribution span value is <1.2.

[0063] Pre-drying:

[0064] Drying in 105°C oven for 2 hours, water content < 0.5%.

[0065] The main components of the obtained soda-lime glass powder are: SiO268-76%, Na2O 11-14%, CaO 9-11%, Fe2O3< 0.05%, MgO 0.8%-1.2%.

[0066] (1.2) Pretreatment of nano-alumina

[0067] Ball-milling dispersion:

[0068] Nano-Al2O3 (particle size 20-50 nm), dispersant, clay, and quartz are added together with water and ball-milled for 4-6 hours (material to water ratio 1:(0.6-1.0)), using zirconia balls as grinding medium, and the size of the final particle agglomerates is controlled to be < 200 nm.

[0069] The dispersant is sodium polyacrylate, and its amount is 0.1-0.5% of the nano-alumina, which reduces the nano-particle agglomeration through chemical bonding.

[0070] (1.3) Treatment of other raw materials

[0071] The specific gravity of kaolin, rongsheng stone powder, ming stone powder, and pressed mud in the raw materials is in the range of 1.5-1.6, the particle size is in the range of 0.5-3 μm, and the shrinkage is in the range of 5.0-7.0%.

[0072] The remaining mineral raw materials are weighed according to the above mass percentage and added to the ball mill tank. After adding ball stones and water, ball milling is performed. The slurry after ball milling is filtered through a screen to remove un-ball-milled particles, dried, and then crushed into powder by a double-roller crusher. The green powder in the size range of 40-60 mesh is separated by a vibrating screen.

[0073] Slurry ball milling coefficient: slurry water content: 39%, ball stone: raw material = 2:1, water surface height: 3 / 5-3 / 4, ball milling time: 15 min, slurry flow rate: 29 s, fineness: 2.13%.

[0074] Green performance parameters: green water content: 6.0-7.0%, green particle size: 40-60 mesh, bulk density: 0.9 g / cm 3 .

[0075] (2) Mixing

[0076] A three-dimensional mixer or a powerful stirrer is used to ensure uniform distribution of nano-AlO and glass powder.

[0077] (2.1) The green powder prepared in step (1.3) is first added to a double-shaft stirrer, and then the pre-dispersed nano-alumina suspension prepared in step (1.2) is slowly added.

[0078] (2.2) Add the sodium-calcium glass powder prepared in step (1.1) and avoid dusting of the light glass powder, and then add the sodium polyacrylate additive.

[0079] (2.3) Start the double shaft mixer.

[0080] Equipment parameters: double shaft mixer, rotation speed 45 rpm, mixing time 30 minutes.

[0081] Additive: sodium polyacrylate as a dispersant, amount 0.1% of the mass of the mineral material.

[0082] Uniformity control: after mixing, take samples for testing, and analyze the composition deviation by XRF, which is ≤2%, and the CV value is <5%.

[0083] (3) Forming and drying

[0084] (3.1) Press forming

[0085] Pressure parameters: use a hydraulic press, press pressure 3200T, pressure holding time 5 seconds.

[0086] Green body density: ≥2.3 g / cm 3 .

[0087] Green body size: short side 675-676 mm, long side 1233-1234 mm, thickness 12.3-12.5 mm.

[0088] (3.2) Drying schedule

[0089] Drying temperature: stepwise drying:

[0090] First stage: 80°C x 30 min (quickly remove surface moisture);

[0091] Second stage: 110°C x 60 min (deep dehydration).

[0092] Moisture content control: after drying, the moisture content of the green body is ≤0.8% (online monitoring by infrared moisture meter).

[0093] (4) Firing process

[0094] The temperature control for firing is shown in Table 1.

[0095] The obtained marble ceramic tile has the following chemical components in mass percentage: SiO2≤67.0%, Al2O3 19.5-20.5%, Fe2O3≤0.8%, CaO≤0.8%, TiO2≤0.2%, MgO 0.7-1.2%, K2O 3.5-4.0%, and Na2O 2.4-2.8%, and the loss on ignition is ≤5.5%.

[0096] Table 1

[0097]

[0098] This invention involves ball milling nano-alumina with clay and quartz from mineral materials, adding a dispersant and water to obtain a nano-alumina suspension, which is then used to prepare marble ceramic tiles, significantly reducing the water absorption rate of the marble ceramic tiles. The highly active nano-alumina fills micropores through surface atomic diffusion and reacts with SiO2 in the clay to form mullite, creating a dense network structure that reduces interconnected pores and grain boundary voids.

[0099] This invention further incorporates sodium-calcium glass powder, which, together with highly active nano-alumina, forms a dual mechanism to synergistically reduce water absorption. Synergistic enhancement effect: The highly active nano-alumina partially dissolves in the glass melt, releasing Al... 3+ With SiO4 in the melt 4- The network combines to form a dense Al-Si-O glass phase, which increases the viscosity of the liquid phase, slows down abnormal grain growth, and maintains the ability of the liquid phase to fill pores.

[0100] Glass powder melts at 1000 degrees Celsius to form a low-viscosity liquid phase, which encapsulates nano-alumina and clay particles. The highly active nano-alumina fills the submicron-level pores, while the glass phase fills the micron-level pores, forming a multi-scale dense structure.

[0101] The amount of sodium-calcium glass powder added should be 2-4%, and the sodium content needs to be controlled to prevent efflorescence later. ≥10% will affect the flatness of the tiles.

[0102] The glass powder must pass through a 325-mesh sieve (D50≤15μm). If it is too coarse (>45μm), it will cause uneven melting in some areas, resulting in spot defects. The moisture content of the glass powder must be ≤0.5% (dried at 105℃ for 2 hours) to avoid moisture fluctuations during the forming of the green body.

[0103] The glass melt alternately penetrates the mullite grain boundaries to form a "glass-mullite" composite phase, which strengthens the interfacial bonding force and reduces microcracks.

[0104] Sodium calcium glass powder stabilizes sodium ions, inhibits efflorescence, and reduces the water absorption rate of ceramic tiles.

[0105] The fluxing effect of calcium sodium glass powder reduces the firing temperature from 1280℃ to about 1230℃, saving about 10-15% of energy.

[0106] This invention improves the flexural strength of ceramic tiles by enhancing the mullitization effect of highly active nano-alumina and the interfacial bonding of the glass phase.

[0107] Examples 1-8 and Comparative Examples 1-4

[0108] The basic raw materials for marble ceramic tiles include minerals, sodium-calcium glass powder, nano-alumina, and dispersants;

[0109] The mineral materials include the following components by mass fraction: Star Potash Sand (Potassium Feldspar) 8 parts, Lusheng Black Slate (Talc, Black Slate) 3 parts, Jintao Stone Powder (Quartz) 14 parts, Rong Sodium Stone Powder (Soda Feldspar) 10 parts, Glaze Mud (Glaze Recycle) 1.0 parts, Edge Mud (Body Recycle) 9 parts, Ming Stone Powder (Zirconium Silicate, Functional Class Raw Material) 14 parts, Rongsheng Stone Powder (Porcelain Stone) 4.5 parts, Squeezed Mud (Recycled Plastic Material) 3 parts, Yanggaili Clay (Kaolin) 8 parts, Yongli Mud (Clay) 8 parts, Huicheng Mud (Clay) 8 parts, Hei Mud (Clay) 4 parts; the components of each mineral material are shown in Table 2.

[0110] Table 2

[0111]

[0112] Marble ceramic tiles were prepared according to the sodium-calcium glass powder and nano-alumina addition amount in Table 5.

[0113] (1) Raw material pretreatment

[0114] (1.1) Sodium-calcium glass powder preparation

[0115] Impurity removal by sorting:

[0116] After crushing, the sodium-calcium glass was removed by color sorter (wavelength 500-600 nm) to remove colored impurities (such as green beer bottle glass), ensuring that the whiteness of the glass powder is >80%.

[0117] Iron removal by magnetic separation:

[0118] Metal impurities were removed using a high-gradient magnetic separator (magnetic field strength 1.2T) to control the Fe2O3 content to ≤0.1%.

[0119] Ultrafine grinding:

[0120] The glass powder was ground using an air jet mill to pass through a 325 mesh screen, with a D50 = 10 μm and a particle size distribution Span value <1.2.

[0121] Pre-drying:

[0122] Drying in a 105°C oven for 2 hours, with a moisture content ≤0.5%.

[0123] The main components of the obtained sodium-calcium glass powder are: SiO2 72%, Na2O 13%, CaO 10%, Fe2O3 0.042%, MgO 1.1%.

[0124] (1.2) Pretreatment of nano-alumina

[0125] Ball milling and dispersion:

[0126] Nano-AlO (particle size 20-50 nm), sodium polyacrylate (0.25 wt% of nano-alumina, to reduce nano-particle agglomeration by chemical bonding) and clay, quartz were ball-milled together for 5.5 hours with water, using zirconium balls as grinding media, to control the final particle agglomerate size < 200 nm.

[0127] The ratio of material to water, dry material: water = 1:0.8; the ratio of balls to material, zirconium balls: dry material = 1.5:1

[0128] The ratio of zirconium ball diameters: Φ3mm: Φ5mm: Φ10mm = 4:3:3.

[0129] (1.3) Other raw material processing

[0130] The specific gravity of the raw materials, kaolin, Rongsheng stone powder, Ming stone powder, and pressed mud, ranges from 1.5 to 1.6, the particle size ranges from 0.5 to 3 μm, and the shrinkage ranges from 5.0 to 7.0%.

[0131] The remaining mineral raw materials were weighed according to the above mass percentage and added to the ball mill tank. After adding the ball stones and water, the slurry was ball-milled, the un-ball-broken particles were filtered out through a screen, and then the dry material was dried and crushed into powder by a double-roller crusher. The green powder with a particle size of 40-60 mesh was separated by a vibrating screen.

[0132] Slurry ball-milling coefficient: slurry moisture content: 39 wt%, ball stones: raw material = 2:1, water surface height: 3 / 5-3 / 4, ball-milling time: 15 min, slurry flow rate: 29 s, fineness: 2.13%.

[0133] Green powder performance parameters: green water content: 7.0%, green particle size: 40-60 mesh, bulk density: 0.9 g / cm 3 .

[0134] (2) Mixing

[0135] (2.1) The green powder prepared in step (1.3) was first added to the double-shaft mixer, and then the pre-dispersed nano-alumina suspension prepared in step (1.2) was slowly added.

[0136] (2.2) The sodium-calcium glass powder prepared in step (1.1) was then added to avoid light dust, followed by the addition of sodium polyacrylate additive.

[0137] (2.3) The double-shaft mixer was started and stirred.

[0138] Equipment parameters: double-shaft mixer, rotation speed 45 rpm, mixing time 30 minutes.

[0139] Additive: 0.1% sodium polyacrylate based on the mass of the mineral material was used as a dispersant.

[0140] Uniformity control: sampling after mixing and detecting the composition deviation by XRF analysis, the value of CV < 5%.

[0141] (3) Shaping and drying

[0142] (3.1) Pressing

[0143] The powder prepared in step 2 was pressed.

[0144] Pressure parameters: using hydraulic press, pressing pressure 3200T, pressure holding time 5 seconds.

[0145] Green body density: ≥ 2.3 g / cm 3 .

[0146] Green body size: short side 675-676 mm, long side 1233-1234 mm, thickness 12.3-12.5 mm.

[0147] (3.2) Drying schedule

[0148] The wet green body prepared in step (3.1) was dried.

[0149] Drying temperature: stepwise drying:

[0150] First stage: 80°C x 30 min (quickly remove surface moisture);

[0151] Second stage: 110°C x 60 min (deep dehydration).

[0152] Moisture content control: the moisture content of the green body after drying ≤ 0.8% (infrared moisture meter online monitoring).

[0153] (4) Firing process

[0154] The dry green body prepared in step (3.2) was fired to obtain marble ceramic tiles.

[0155] Firing temperature as shown in Table 3.

[0156] The chemical composition of the marble ceramic tiles prepared is: SiO2≤ 67.0%, Al2O3 19.5-20.5%, Fe2O3≤ 0.8%, CaO≤ 0.8%, TiO2≤ 0.2%, MgO 0.7-1.2%, K2O 3.5-4.0%, and Na2O 2.4-2.8%, and the loss on ignition is ≤ 5.5%.

[0157] Table 3

[0158]

[0159] Comparative Example 5

[0160] Step (1.2) and step (1.3) are as follows, and other steps are the same as Example 1.

[0161] (1.2) Pretreatment of nano-alumina

[0162] Ball-milling dispersion:

[0163] Nano-Al2O3 (particle size 20-50 nm), sodium polyacrylate (0.25 wt% of nano-alumina, to reduce nano-particle agglomeration by chemical bonding) were added to water and ball-milled for 5.5 hours, using zirconium balls as the grinding medium.

[0164] The ratio of material to water, dry material: water = 1:0.8; the ratio of balls to material, zirconium balls: dry material = 1.5:1

[0165] The ratio of zirconium ball diameters: Φ3mm: Φ5mm: Φ10mm = 4:3:3.

[0166] (1.3) Treatment of other raw materials

[0167] In the raw materials, kaolin, jintao stone powder, rongsheng stone powder, ming stone powder, and pressed mud have a specific gravity range of 1.5-1.6, a particle size range of 0.5-3 μm, and a shrinkage range of 5.0-7.0%.

[0168] Each mineral raw material was weighed according to the above mass percentage and added to the ball mill tank. After adding the ball stones and water, ball milling was performed. The well-milled slurry was filtered through a screen to remove un-ball-milled particles, then dried, and then ground into powder by a double-roller crusher. The 40-60 mesh interval of the blank powder was separated by a vibrating screen.

[0169] Slurry ball milling coefficient: slurry moisture content: 39 wt%, ball stones: raw material = 2:1, water surface height: 3 / 5-3 / 4, ball milling time: 15 min, slurry flow rate: 29 s, fineness: 2.13%.

[0170] Blank powder performance parameters: blank moisture: 7.0%, blank particle size: 40-60 mesh, bulk density: 0.9 g / cm 3 .

[0171] The marble ceramic tiles prepared in Examples 1-8 and Comparative Examples 1-5 were subjected to performance testing, and the quality detection methods and standards are shown in Table 4, and the detection results are shown in Table 5.

[0172] Table 4

[0173]

[0174] Table 5

[0175]

[0176] Note: Oxygen represents nano-alumina, and glass represents soda-lime glass powder.

[0177] As can be seen from Table 5:

[0178] Comparative Example 5 directly added nano-alumina, which can reduce the water absorption rate to a certain extent; Example 1 can significantly reduce the water absorption rate after adjusting the process;

[0179] Examples 3-8 further significantly reduced the water absorption rate after adding soda-lime glass powder, especially Example 7, with a water absorption rate of only 0.05%, and at the same time, good glazing effect, high flexural strength and low alkali precipitation.

[0180] Example 7 is used to illustrate the synergistic effect of nano-alumina and soda-lime glass powder in reducing water absorption. Comparative Example 3 only added 4% soda-lime glass powder, which reduced the water absorption rate by 33.9% (1-0.39 / 0.59), and Example 2 only added 2% nano-alumina, which reduced the water absorption rate by 59.3%. In theory, if 4% soda-lime glass powder and 2% nano-alumina are added at the same time, the water absorption rate will be reduced by 1-(1-33.9%)*(1-59.3%) = 73.1%, and the actual water absorption rate of Example 7 of the present application is reduced by 91.5%. It can be seen that nano-alumina and soda-lime glass powder have a synergistic effect in reducing water absorption.

[0181] The above is a specific description of the preferred implementation of the present application, but the present application is not limited to the described embodiments. Those skilled in the art can make various equivalent modifications or substitutions without departing from the spirit of the present application. These equivalent modifications or substitutions are all included in the scope defined by the claims of the present application.

Claims

1. A method for preparing marble ceramic tiles with low water absorption, characterized in that, Includes the following steps: (1) Nano alumina, dispersant and clay and quartz in mineral materials are ball-milled together with water to obtain nano alumina suspension; (2) Add water to the potassium feldspar, black talc, sodium feldspar, glaze recycled material, body recycled material, zirconium silicate, porcelain stone, recycled plastic material and kaolin in the ore, ball mill, dry and crush to obtain body powder. (3) Add the nano alumina suspension from step (1) to the blank powder from step (2), then add sodium calcium glass powder and dispersant, stir, press into shape, dry, and fire to obtain marble ceramic tiles with low water absorption. The raw materials for the low water absorption marble ceramic tile include minerals, sodium-calcium glass powder, nano-alumina, and dispersants. By weight, the mineral material includes the following components: 6.0-10.0 parts potassium feldspar, 1.0-4.5 parts black talc, 12-16 parts quartz, 8-12 parts sodium feldspar, 1.0-1.5 parts recycled glaze, 6-12 parts recycled body material, 10-16 parts zirconium silicate, 4.5-6 parts porcelain stone, 3-4 parts recycled plastic material, 5-10 parts kaolin, and 17-24 parts clay. The amount of sodium-calcium glass powder used is 0% to 6% of the mineral mass; The amount of nano-alumina used is 1% to 3% of the mineral mass; The amount of dispersant used in step (1) is 0.1% to 0.5% of the mass of nano-alumina; The amount of dispersant used in step (3) is 0.05% to 0.2% of the mineral mass.

2. The preparation method according to claim 1, characterized in that, The amount of sodium-calcium glass powder used is 2% to 6% of the mineral mass; The amount of nano-alumina used is 1% to 2% of the mineral mass.

3. The preparation method according to claim 2, characterized in that, The amount of sodium-calcium glass powder used is 2% to 4% of the mass of the mineral. The amount of nano-alumina used is 1% to 2% of the mineral mass.

4. The preparation method according to claim 1, characterized in that, By weight, the mineral material includes the following components: 6.0-10.0 parts of Xingchen potassium sand, 1.0-4.5 parts of Lusheng black talc, 12-16 parts of Jintao stone powder, 8-12 parts of Rongna stone powder, 1.0-1.5 parts of glaze clay, 6-12 parts of grinding clay, 10-16 parts of Ming stone powder, 4.5-6 parts of Rongsheng stone powder, 3-4 parts of pressed clay, 5-10 parts of Yangkaolin clay, 7-9 parts of Yongli clay, 7-9 parts of Huaicheng clay, and 3-6 parts of Fei clay.

5. The preparation method according to claim 1, characterized in that, In step (1), the particle size of the nano-alumina is 20-50 nm; In step (1), the dispersant is sodium polyacrylate; In step (1), the time for ball milling with water is 4 to 6 hours, and the material-to-water ratio for ball milling with water is 1:(0.6-1.0).

6. The preparation method according to claim 1, characterized in that, In step (2), the material-to-water ratio for ball milling is (60-65):(35-40), and the time is 10-20 min; In step (2), the moisture content of the obtained raw material powder is 5% to 7.0%, and the particle size is 40 to 60 mesh.

7. The preparation method according to claim 1, characterized in that, In step (3), the particle size of the soda-lime glass powder is D50 = 10-15 μm; In step (3), the composition of the sodium-calcium glass powder is: SiO2 68-76%, Na2O 11-14%, CaO 9-11%, Fe2O3≤0.05%, MgO 0.8%-1.2%, and the remainder is other components.

8. The preparation method according to claim 1, characterized in that, In step (3), the dispersant is sodium polyacrylate; In step (3), the stirring speed is 45-60 rpm and the time is 30-60 minutes; In step (3), the pressing pressure is 3200-3500T, and the holding time is 5-10 seconds; In step (3), the moisture content of the dried green body is ≤0.8%; In step (3), the firing parameters are as follows: heating from room temperature to 600℃ at a heating rate of 20-50℃ / min, heating from 600℃ to 1000℃ at a heating rate of 60-70℃ / min, heating from 1000℃ to 1230℃ at a heating rate of 50-60℃ / min, holding at 1230℃ for 15-20min, cooling from 1230℃ to 600℃ at a cooling rate of 120-150℃ / min, and cooling from 600℃ to room temperature at a cooling rate of 20-30℃ / min.

9. The preparation method according to claim 1, characterized in that, In step (3), after drying and before firing, surface glaze is applied, inkjet printing is performed, and protective glaze is applied.

10. Marble ceramic tiles with low water absorption rate prepared by the preparation method according to any one of claims 1-9.

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