A super three-dimensional penetrating flower glaze and its preparation process

Abstract

The present invention relates to a super-stereoscopic penetrating flower glaze and its preparation process, belonging to the technical field of ceramic glaze preparation. In the present invention, the vitrification degree of the glaze is improved by modifying potassium feldspar. Magnesium chloride and calcium nitrate are introduced through grinding to form a new complex, and chemical adsorption occurs on the surface of the potassium feldspar complex through treatment with boric acid solution and CTAB solution, forming a new interfacial layer, enabling the potassium feldspar complex to reach a molten state at a lower temperature; the silane coupling agent forms an organic layer on the surface of talc powder through chemical action, which helps to optimize the structure of the glaze layer and promote the sintering process, reducing the required formulation temperature and making the obtained glaze layer have better wear resistance; in the present invention, the rigidity of the hard module and the flexibility of the elastic module are combined. After the hard module treatment, the elastic module is used for supplementary polishing, making the obtained super-stereoscopic penetrating flower glaze finished product have better texture.

Description

Technical Field

[0001] The present invention belongs to the technical field of ceramic glaze preparation, and relates to a super three-dimensional penetrating glaze and a preparation process thereof. Background Art

[0002] Penetrating tiles combine the wear resistance, corrosion resistance, high strength of granite and the decorative effect of rich colors, and have become one of the indispensable leading products in building decoration materials. With the continuous development of technology, the consumption level and aesthetic level are constantly improving, and people's requirements for the decorative effect of penetrating polished tiles are also constantly increasing. At present, in the traditional preparation method of penetrating tiles, the texture pattern on its surface can only print water-soluble penetrating ink on the surface slurry poured on the blank body by printing. The three-dimensional sense of the tiles is insufficient, and only a decorative pattern with a certain depth is generated on the surface of the tiles after penetration. In the subsequent polishing process, it is necessary to accurately control the polishing amount to ensure that the decorative pattern on the surface of the penetrated tiles is not polished away. In actual operation, it is necessary to conduct multiple tests to determine the polishing amount, which consumes time and cost.

[0003] The purpose of the present invention is to provide a process and preparation method for a super three-dimensional penetrating glaze material, which can realize the cloth laying of different texture blanks according to the inkjet penetrating pattern, improve the overall three-dimensional sense of the penetrating tiles, and at the same time avoid the phenomenon of bottom penetration of the penetrating tiles, overcoming the deficiencies in the prior art. Summary of the Invention

[0004] The purpose of the present invention is to provide a super three-dimensional penetrating glaze and a preparation process thereof, which have the characteristics of wear resistance and stain resistance.

[0005] The purpose of the present invention can be realized by the following technical solutions:

[0006] A super three-dimensional penetrating glaze, the raw materials of the penetrating glaze include glaze A and glaze B,

[0007] The raw materials of glaze A are as follows, by mass percentage, 30-35% of modified potassium feldspar, 40-45% of albite, 3-5% of kaolin, 2-4% of ball clay, 5-10% of quartz, and 10-15% of fused quartz;

[0008] Among them, the preparation method of modified potassium feldspar is:

[0009] S11: Mix potassium feldspar, magnesium chloride and calcium nitrate in a mass ratio of (3-5):1:1, and grind in a ball mill at a speed of 400 r / min for 1 h to obtain mixture A;

[0010] S12: Disperse mixture A in boric acid solution to obtain a solid-liquid mixture B with a mass fraction of 20-30%. After ultrasonic treatment for 0.5 h, filter and dry at 110 °C for 8 h to obtain mixture C;

[0011] S13: Disperse mixture C in a cetyltrimethylammonium bromide (CTAB) solution with a mass fraction of 20%, where the mass ratio of mixture C to CTAB is 1:(1 - 3). Sonicate for 0.5 h, filter, and dry at 80°C for 12 h. Then, heat the dried mixture in a muffle furnace from room temperature to 400°C and calcine for 3 h. After calcination, cool and grind to a particle size of 300 mesh to obtain the modified potassium feldspar;

[0012] The raw materials of glaze B are as follows, by mass percentage: potassium feldspar 30 - 35%, albite 30 - 40%, kaolin 3 - 5%, ball clay 2 - 4%, quartz 10 - 15%, fused quartz 10 - 15%, and modified talc powder 2 - 5%;

[0013] Among them, the preparation method of the modified talc powder is as follows:

[0014] S21: Put talc into a ball mill and grind at a speed of 400 r / min for 1 h to obtain talc powder with a particle size of 200 mesh;

[0015] S22: Dissolve the silane coupling agent in deionized water to prepare a silane coupling agent solution with a mass fraction of 30 - 50%. Disperse the talc powder obtained by grinding in S21 in the silane coupling agent solution, where the mass ratio of talc powder to silane coupling agent is 1:1 to obtain a solid-liquid mixture D;

[0016] S23: Heat the solid-liquid mixture D to 40°C, stir at a speed of 150 - 200 r / min for 1 - 2 h. After stirring, sonicate for 0.5 h. After sonication, filter and dry at 80°C for 12 h. Then, grind again, with the ball mill speed at 500 r / min and the grinding time at 2 h to obtain the modified talc powder.

[0017] Furthermore, the mass fraction of the boric acid solution in S12 is 10 - 15%.

[0018] Furthermore, the heating rate of the muffle furnace in S13 is 5°C / min.

[0019] Furthermore, the particle size of the modified talc powder obtained by grinding in S23 is 300 mesh.

[0020] A preparation process of a super three-dimensional penetrating flower glaze. The specific process flow of the preparation process of the super three-dimensional penetrating flower glaze is as follows.

[0021] S51: Put the raw materials of glaze A into a ball mill according to the formula ratio. The rotation speed of the ball mill is 300 r / min. After grinding for 1 h, add 40 wt% of water, 0.1 wt% of sodium carboxymethyl cellulose, and 0.4 wt% of sodium tripolyphosphate. Increase the rotation speed of the ball mill to 500 r / min and continue grinding for 8 h. Use a magnetic iron remover to remove iron to obtain glaze A;

[0022] S52: Put the raw materials of glaze B into a ball mill according to the formula ratio. The rotation speed of the ball mill is 300 r / min. After grinding for 1 h, add 40 wt% of water, 0.1 wt% of sodium carboxymethyl cellulose, and 0.4 wt% of sodium tripolyphosphate. Increase the rotation speed of the ball mill to 500 r / min and continue grinding for 8 h. Use a magnetic iron remover to remove iron to obtain glaze B;

[0023] S53: Purge the surface of the green body with nitrogen. First, pour glaze A on the surface of the green body by the glazing method. After pouring, let it stand for drying to obtain green body Ⅰ;

[0024] S54: Pour glaze B on the surface of green body Ⅰ by the glazing method. After pouring, put it into a drying kiln of the glaze line for drying. The temperature of the drying kiln is 200 °C to obtain green body Ⅱ;

[0025] S55: Print the inlaid pattern ink on the surface of green body Ⅱ. After printing, directly put it into a kiln for firing. The temperature of the kiln is 1160 °C, and the firing cycle is 65 min. After firing, cool it to room temperature to obtain a semi-finished product;

[0026] S56: Polish the semi-finished product obtained in S55 to obtain the super three-dimensional inlaid pattern glaze.

[0027] Further, the purging flow rate of nitrogen in S53 is 8 m / s.

[0028] Further, the parameters of the glazing method in S53 are as follows: the glazing distance is 25 cm, the specific gravity of glaze A is 1.83 - 1.86 g / ml, the glazing amount is 70 g / piece, and the size of the brick piece is 300 * 600 mm.

[0029] Further, the parameters of the glazing method in S54 are as follows: the glazing distance is 25 cm, the specific gravity of glaze B is 1.83 - 1.86 g / ml, the glazing amount is 80 g / piece, and the size of the brick piece is 300 * 600 mm.

[0030] Further, the polishing treatment in S56 is carried out successively using the following grinding heads: a grinding head composed of 5 groups of 100-mesh hard modules, a grinding head composed of 4 groups of 600-mesh elastic modules, a grinding head composed of 4 groups of 800-mesh elastic modules, a grinding head composed of 5 groups of 1500-mesh elastic modules, and a grinding head composed of 4 groups of 2000-mesh elastic modules.

[0031] Further, in S56, the pressure exerted by the grinding head of the hard grinding block during polishing on the tile surface is 1.5 MPa, and the pressure exerted by the grinding head composed of elastic modules on the tile surface is 0.3 - 0.5 MPa.

[0032] In the formulas of the penetrating decorative glazes A and B, the main functions of potassium feldspar and sodium feldspar are fluxes to increase the vitrification degree of the glaze. The main function of quartz is to improve the mechanical strength of the glaze layer. The main function of fused quartz is to reduce the expansion coefficient. Kaolin improves the suspension of the glaze slurry. Ball clay improves the fluidity of the glaze slurry, prevents the glaze slurry from thixotropy, and the main function of talc is to reduce the formula temperature.

[0033] Glaze A is directly poured on the green body as the base glaze. Its main function is to make the combination between the green body and the surface glaze more firm. This adhesion effect ensures the stability and durability of the glaze layer on the ceramic product, preventing the glaze layer from peeling off or flaking during use, which makes the ceramic product more durable during use and able to resist external force impacts and abrasions. The base glaze can also be used to cover the color, defects, roughness or exposed harmful minerals on the surface of the green body. By applying the base glaze, the surface of the ceramic product can be made more flat and smooth, improving the aesthetics of the product.

[0034] As a basic glaze, the base glaze can also enhance the toughness and wear resistance of the ceramic product. In the present invention, potassium feldspar in the base glaze is modified to further improve the vitrification degree of the glaze. Vitrification is the process in which the glaze layer melts and recrystallizes at high temperature to form a vitreous glaze surface. This glaze surface has high strength and hardness, which can effectively improve the overall mechanical properties of the ceramic product, making it more wear-resistant and impact-resistant. As the vitrification degree of the base glaze increases, the density of the glaze layer also increases, thereby reducing the water absorption rate of the ceramic product. A low water absorption rate means that the ceramic product can better resist water penetration during use, reducing problems such as expansion and cracking caused by water absorption. The vitrified glaze layer has better chemical stability and can resist the corrosion of gases, liquids, acids and alkalis and other chemical substances.

[0035] In the present invention, potassium feldspar is mixed with magnesium chloride and calcium nitrate and ground. During the grinding process, the crystal structure of potassium feldspar will be damaged to a certain extent, making the elements such as potassium, aluminum, and silicon inside it more active and easier to react with other components. Therefore, the introduction of magnesium chloride and calcium nitrate can form a new complex, and the newly formed complex has better fusibility and stability; the treatment in boric acid solution and CTAB solution causes chemical adsorption on the surface of the potassium feldspar complex, forming a new interfacial layer. This interfacial layer has better wettability and dispersibility, which helps to be evenly distributed in the glaze. As a cationic surfactant, CTAB can also be adsorbed on the surface of potassium feldspar through electrostatic interaction, forming a stable coating layer to prevent the aggregation and precipitation of potassium feldspar particles; boric acid, as a glass former, can effectively reduce the melting temperature of the glaze. During the modification process, the addition of boric acid enables the potassium feldspar complex to reach the molten state at a lower temperature, thereby promoting the formation and vitrification of the glaze layer.

[0036] Potassium feldspar itself has a relatively high melting viscosity, and the modified potassium feldspar complex further enhances this property. The high-viscosity melt is more likely to form a dense and uniform glass phase during the cooling process, thereby improving the vitrification degree of the glaze; the elements such as potassium, aluminum, and silicon in the modified potassium feldspar can undergo chemical reactions with quartz in the formula during the melting process to form a stable glass phase. These glass phases can firmly adhere to the ceramic body after cooling, forming a smooth and hard glaze layer.

[0037] Glaze B is then poured as the top glaze outside Glaze A. The smoothness and gloss of the top glaze can significantly improve the texture of the ceramic product. The dense structure and chemical stability of the top glaze endow it with excellent stain resistance. It can effectively prevent pollutants such as stains and oil stains from penetrating into the ceramic interior, keeping the product clean and hygienic; the top glaze can resist the erosion of chemical substances such as acids, alkalis, and salts, protecting the ceramic product from damage. The top glaze can also improve the thermal stability of the ceramic product, making it not easy to deform or crack in a high-temperature environment. This is particularly important for ceramic products that need to withstand high temperatures. The reduction of the top glaze formula temperature means less energy is required during the firing process. The firing of ceramic products in a kiln is a high-energy-consuming process. Reducing the top glaze formula temperature can significantly reduce energy consumption and production costs. Excessive firing temperature may cause the ceramic product to deform or crack due to uneven thermal stress during the firing process. Therefore, reducing the top glaze formula temperature also helps the top glaze to form a uniform and dense glaze layer on the ceramic surface. This can not only improve the aesthetics of the product but also enhance the wear resistance, corrosion resistance, and other properties of the glaze surface. In the present invention, a silane coupling agent is used to modify talc to further reduce the top glaze formula temperature during the preparation process.

[0038] Silane coupling agents are a class of low-molecular-weight organosilicon compounds with special structures, and their general chemical formula is usually RSiX 3 , where X represents a hydrolyzable group, and R represents an active functional group that has an affinity or reactivity with polymer molecules. When the silane coupling agent is mixed with talc powder and heated, the X groups in the silane coupling agent will first undergo a hydrolysis reaction to generate silanols (Si-OH). Further condensation reactions will occur between the generated silanols to form oligomeric siloxanes (Si-O-Si). These oligomeric siloxanes have a network structure. The Si-OH groups of the oligomeric siloxanes will react with the hydroxyl groups (OH) on the surface of the talc powder to form hydrogen bonds and dehydrate and solidify during further heating, ultimately forming strong covalent bonds (Si-O-M, where M represents metal ions or groups on the surface of the talc powder). The silane coupling agent (KH-570) used in this invention is purchased from Sinopharm Chemical Reagent Co., Ltd.

[0039] The dispersibility of talc powder modified by the silane coupling agent in the glaze is significantly improved. Since an organic layer is formed on the surface of the talc powder by the silane coupling agent, this organic layer has better compatibility with the organic substances in the glaze, thereby reducing the agglomeration phenomenon between talc powder particles and enabling the talc powder to be more evenly dispersed in the glaze; due to the improved dispersibility of the talc powder in the glaze, the contact area between the talc powder particles and other components in the glaze increases, which helps to accelerate the mass diffusion and chemical reactions during the sintering process. Therefore, under the same sintering conditions, the modified talc powder can more effectively promote the sintering process of the glaze, thereby potentially reducing the required sintering temperature; a strong chemical bonding is formed between the talc powder modified by the silane coupling agent and the organic substances in the glaze, and this bonding effect helps to form a denser and more uniform structure in the glaze layer and also gives the prepared glaze layer better wear resistance.

[0040] In order to make the finished product of the super three-dimensional penetrating flower glaze have a better texture, its surface is polished after firing. In the present invention, the rigidity of the hard module and the flexibility of the elastic module are combined. When using the hard module alone for polishing, due to its high hardness, it may cause certain damage to the glaze surface, such as scratches or microcracks. After the hard module treatment, the elastic module is used for supplementary polishing, which can effectively reduce these damages. The flexibility of the elastic module can avoid further scratches or damages to the glaze surface, and at the same time can fill and repair the tiny defects that may occur during the hard module treatment process. In the present invention, the pressure exerted by the grinding head of the hard grinding block on the tile surface is 1.5 MPa, and the pressure exerted by the grinding head composed of the elastic module on the tile surface is 0.3 - 0.5 MPa. If the pressure exerted by the hard grinding head on the glaze surface is too large, resulting in too much shaving amount, it will cause excessive polishing of the glaze surface and expose the bottom blank, resulting in defects. If the pressure exerted by the grinding head on the glaze surface is too small, resulting in too little shaving amount, the flatness of the polished glaze surface is not good and the surface layer effect is poor, with more dot-like crystals and less flash of surface-like crystals.

[0041] Advantages of the present invention:

[0042] (1) In the present invention, the vitrification degree of the glaze is improved by modifying potassium feldspar. Magnesium chloride and calcium nitrate are introduced through grinding to form a new complex. The newly formed complex has better fluxing property and stability, and through the treatment in boric acid solution and CTAB solution, chemical adsorption occurs on the surface of the potassium feldspar complex, forming a new interfacial layer, making the potassium feldspar complex have better wettability and dispersibility and being not easy to agglomerate and precipitate, and enabling the potassium feldspar complex to reach the molten state at a lower temperature, thus promoting the formation and vitrification of the glaze layer;

[0043] (2) The silane coupling agent forms an organic layer on the surface of talc powder through chemical action, improving the dispersibility of talc powder in the glaze and its compatibility with organic substances. At the same time, this modification also helps to optimize the structure of the glaze layer and promote the sintering process, thereby reducing the required formulation temperature and making the prepared glaze layer have better wear resistance;

[0044] (3) In the present invention, the rigidity of the hard module and the flexibility of the elastic module are combined. After the hard module treatment, the elastic module is used for supplementary polishing to make the finished product of the super three-dimensional penetrating flower glaze have a better texture. Description of the drawings

[0045] For the convenience of those skilled in the art to understand, the present invention will be further described below with reference to the drawings.

[0046] Figure 1 Effect diagram of the super three-dimensional penetrating flower glaze prepared in Example 1 of the present invention. Detailed implementation manners

[0047] To further elaborate on the technical means and effects adopted by the present invention to achieve the intended invention purpose, the following, in combination with the accompanying drawings and preferred embodiments, details the specific implementation manners, structures, features and their effects of the present invention as follows.

[0048] Example 1

[0049] The formula of glaze A is as follows. By mass percentage, modified potassium feldspar is 35%, albite is 40%, kaolin is 5%, ball clay is 4%, quartz is 6%, and fused quartz is 10%.

[0050] The preparation method of the modified potassium feldspar is as follows:

[0051] S11: Mix potassium feldspar, magnesium chloride and calcium nitrate in a mass ratio of 4:1:1, grind in a ball mill at a rotation speed of 400 r / min for 1 h to obtain mixture A;

[0052] S12: Disperse mixture A in boric acid solution with a mass fraction of 15% to prepare a solid-liquid mixture B with a mass fraction of 25%. After ultrasonic treatment for 0.5 h, filter and dry at 110 °C for 8 h to obtain mixture C;

[0053] S13: Disperse mixture C in a cetyltrimethylammonium bromide CTAB solution with a mass fraction of 20%, where the mass ratio of mixture C to CTAB is 1:2. After ultrasonic treatment for 0.5 h, filter and dry at 80 °C for 12 h. Then heat the dried mixture in a muffle furnace from room temperature to 400 °C and calcine for 3 h. The heating rate of the muffle furnace is 5 °C / min. After calcination, cool and grind to a particle size of 300 mesh to obtain the modified potassium feldspar;

[0054] The formula of glaze B is as follows. By mass percentage, potassium feldspar is 30%, albite is 35%, kaolin is 3%, ball clay is 2%, quartz is 10%, fused quartz is 15%, and modified talc powder is 5%;

[0055] The preparation method of the modified talc powder is as follows:

[0056] S21: Put talc into a ball mill and grind at a rotation speed of 400 r / min for 1 h to obtain talc powder with a particle size of 200 mesh;

[0057] S22: Dissolve silane coupling agent KH-570 in deionized water to prepare a silane coupling agent solution with a mass fraction of 50%. Disperse the talc powder ground in S21 in the silane coupling agent solution, where the mass ratio of talc powder to silane coupling agent is 1:1, to obtain a solid-liquid mixture D;

[0058] S23: Heat the solid-liquid mixture D to 40°C, stir at a rotation speed of 200 r / min for 2 h, then ultrasonicate for 0.5 h after stirring is completed. After ultrasonication, filter and dry at 80°C for 12 h. After drying, grind again. The rotation speed of the ball mill is 500 r / min and the grinding duration is 2 h to obtain the modified talc powder. The particle size of the obtained modified talc powder is 300 mesh.

[0059] A preparation process of a super three-dimensional penetrating flower glaze. The specific process flow of the preparation process of the super three-dimensional penetrating flower glaze is as follows.

[0060] S51: Put the raw materials of glaze A into a ball mill according to the formula ratio. The rotation speed of the ball mill is 300 r / min. After grinding for 1 h, add 40 wt% of water, 0.1 wt% of sodium carboxymethylcellulose and 0.4 wt% of sodium tripolyphosphate. Increase the rotation speed of the ball mill to 500 r / min and continue grinding for 8 h. Use a magnetic iron remover to remove iron to obtain glaze A.

[0061] S52: Put the raw materials of glaze B into a ball mill according to the formula ratio. The rotation speed of the ball mill is 300 r / min. After grinding for 1 h, add 40 wt% of water, 0.1 wt% of sodium carboxymethylcellulose and 0.4 wt% of sodium tripolyphosphate. Increase the rotation speed of the ball mill to 500 r / min and continue grinding for 8 h. Use a magnetic iron remover to remove iron to obtain glaze B.

[0062] S53: Purge the surface of the green body with nitrogen. The purging flow rate of nitrogen is 8 m / s. First, pour glaze A on the surface of the green body by the glaze pouring method. The parameters of the glaze pouring method are as follows: the glaze pouring distance is 25 cm, the specific gravity of glaze A is 1.86 g / ml, the glaze application amount is 70 g / piece, the size of the brick piece is 300*600 mm. After pouring is completed, let it stand and dry to obtain green body I.

[0063] S54: Pour glaze B on the surface of green body I by the glaze pouring method. The parameters of the glaze pouring method are as follows: the glaze pouring distance is 25 cm, the specific gravity of glaze B is 1.86 g / ml, the glaze application amount is 80 g / piece, the size of the brick piece is 300*600 mm. After pouring is completed, put it into a glaze line drying kiln for drying. The temperature of the drying kiln is 200°C to obtain green body II.

[0064] S55: Print penetrating flower ink on the surface of green body II. After printing, directly put it into a kiln for firing. The temperature of the kiln is 1160°C and the firing cycle is 65 min. After firing, cool it to room temperature to obtain a semi-finished product.

[0065] S56: The semi-finished product obtained in S55 is polished. The polishing process is carried out successively using the following grinding heads: a grinding head composed of 5 groups of 100-mesh hard modules, a grinding head composed of 4 groups of 600-mesh elastic modules, a grinding head composed of 4 groups of 800-mesh elastic modules, a grinding head composed of 5 groups of 1500-mesh elastic modules, and a grinding head composed of 4 groups of 2000-mesh elastic modules. The pressure exerted by the grinding head with hard grinding blocks on the tile surface is 1.5 MPa, and the pressure exerted by the grinding heads composed of elastic modules on the tile surface is 0.4 MPa, obtaining the super three-dimensional penetrating flower glaze.

[0066] Example 2

[0067] The formula of glaze A is as follows. By mass percentage, modified potassium feldspar is 30%, albite is 45%, kaolin is 3%, ball clay is 2%, quartz is 5%, and fused quartz is 15%.

[0068] The preparation method of modified potassium feldspar is:

[0069] S11: Potassium feldspar, magnesium chloride, and calcium nitrate are mixed at a mass ratio of 3:1:1, and ground in a ball mill at a rotation speed of 400 r / min for 1 h to obtain mixture A.

[0070] S12: Mixture A is dispersed in a boric acid solution with a mass fraction of 10% to prepare a solid-liquid mixture B with a mass fraction of 30%. After ultrasonic treatment for 0.5 h, it is filtered and dried at 110 °C for 8 h to obtain mixture C.

[0071] S13: Mixture C is dispersed in a cetyltrimethylammonium bromide (CTAB) solution with a mass fraction of 20%, where the mass ratio of mixture C to CTAB is 1:1. After ultrasonic treatment for 0.5 h, it is filtered and dried at 80 °C for 12 h. The dried mixture is calcined in a muffle furnace from room temperature to 400 °C at a heating rate of 5 °C / min for 3 h. After the calcination is completed, it is cooled and ground to a particle size of 300 mesh to obtain the modified potassium feldspar.

[0072] The formula of glaze B is as follows. By mass percentage, potassium feldspar is 30%, albite is 40%, kaolin is 3%, ball clay is 2%, quartz is 10%, fused quartz is 13%, and modified talc powder is 2%.

[0073] The preparation method of modified talc powder is:

[0074] S21: Talc is put into a ball mill and ground at a rotation speed of 400 r / min for 1 h to obtain talc powder with a particle size of 200 mesh.

[0075] S22: Dissolve the silane coupling agent KH-570 in deionized water to prepare a silane coupling agent solution with a mass fraction of 30%. Disperse the talcum powder obtained by grinding in S21 in the silane coupling agent solution, where the mass ratio of talcum powder to silane coupling agent is 1:1, to obtain a solid-liquid mixture D;

[0076] S23: Heat the solid-liquid mixture D to 40 °C, stir at a speed of 200 r / min for 1 h, then perform ultrasonic treatment for 0.5 h after stirring. After the ultrasonic treatment, filter and dry at 80 °C for 12 h. After drying, grind again. The speed of the ball mill is 500 r / min, and the grinding time is 2 h to obtain the modified talcum powder. The particle size of the obtained modified talcum powder is 300 mesh.

[0077] A preparation process of a super three-dimensional penetrating flower glaze, the specific process flow of the preparation process of the super three-dimensional penetrating flower glaze is as follows.

[0078] S51: Put the raw materials of glaze A into a ball mill according to the formula ratio. The speed of the ball mill is 300 r / min. After grinding for 1 h, add 40 wt% of water, 0.1 wt% of sodium carboxymethyl cellulose, and 0.4 wt% of sodium tripolyphosphate. Increase the speed of the ball mill to 500 r / min and continue grinding for 8 h. Use a magnetic iron remover to remove iron to obtain glaze A;

[0079] S52: Put the raw materials of glaze B into a ball mill according to the formula ratio. The speed of the ball mill is 300 r / min. After grinding for 1 h, add 40 wt% of water, 0.1 wt% of sodium carboxymethyl cellulose, and 0.4 wt% of sodium tripolyphosphate. Increase the speed of the ball mill to 500 r / min and continue grinding for 8 h. Use a magnetic iron remover to remove iron to obtain glaze B;

[0080] S53: Blow the surface of the green body with nitrogen. The blowing flow rate of nitrogen is 8 m / s. First, pour glaze A on the surface of the green body by the glaze pouring method. The parameters of the glaze pouring method are: the glaze pouring distance is 25 cm, the specific gravity of glaze A is 1.83 g / ml, the glazing amount is 70 g / piece, the size of the brick piece is 300*600 mm. After pouring, let it stand and dry to obtain green body Ⅰ;

[0081] S54: Pour glaze B on the surface of green body Ⅰ by the glaze pouring method. The parameters of the glaze pouring method are: the glaze pouring distance is 25 cm, the specific gravity of glaze B is 1.83 g / ml, the glazing amount is 80 g / piece, the size of the brick piece is 300*600 mm. After pouring, put it into a glaze line drying kiln for drying. The temperature of the drying kiln is 200 °C to obtain green body Ⅱ;

[0082] S55: Print penetrating flower ink on the surface of green body Ⅱ. After printing, directly put it into a kiln for firing. The temperature of the kiln is 1160 °C, and the firing cycle is 65 min. After firing, cool it to room temperature to obtain a semi-finished product;

[0083] S56: The semi-finished product obtained in S55 is polished. The polishing process is carried out successively using the following grinding heads: a grinding head composed of 5 groups of 100-mesh hard modules, a grinding head composed of 4 groups of 600-mesh elastic modules, a grinding head composed of 4 groups of 800-mesh elastic modules, a grinding head composed of 5 groups of 1500-mesh elastic modules, and a grinding head composed of 4 groups of 2000-mesh elastic modules. The pressure exerted on the tile surface by the grinding head with hard grinding blocks is 1.5 MPa, and the pressure exerted on the tile surface by the grinding heads composed of elastic modules is 0.3 MPa each, obtaining the super three-dimensional penetrating flower glaze.

[0084] Example 3

[0085] The formula of glaze A is as follows, by mass percentage: modified potassium feldspar 30%, albite 40%, kaolin 3%, ball clay 2%, quartz 10%, fused quartz 15%;

[0086] The preparation method of modified potassium feldspar is:

[0087] S11: Potassium feldspar, magnesium chloride and calcium nitrate are mixed in a mass ratio of 5:1:1, and ground in a ball mill at a rotation speed of 400 r / min for 1 h to obtain mixture A;

[0088] S12: Mixture A is dispersed in boric acid solution with a mass fraction of 15% to prepare a solid-liquid mixture B with a mass fraction of 20%. After ultrasonic treatment for 0.5 h, it is filtered and dried at 110 °C for 8 h to obtain mixture C;

[0089] S13: Mixture C is dispersed in cetyltrimethylammonium bromide CTAB solution with a mass fraction of 20%, where the mass ratio of mixture C to CTAB is 1:3. After ultrasonic treatment for 0.5 h, it is filtered and dried at 80 °C for 12 h. The dried mixture is calcined in a muffle furnace from room temperature to 400 °C for 3 h, and the heating rate of the muffle furnace is 5 °C / min. After calcination, it is cooled and ground to a particle size of 300 mesh to obtain the modified potassium feldspar;

[0090] The formula of glaze B is as follows, by mass percentage: potassium feldspar 30%, albite 30%, kaolin 5%, ball clay 4%, quartz 15%, fused quartz 13%, modified talc powder 3%;

[0091] The preparation method of modified talc powder is:

[0092] S21: Talc is put into a ball mill and ground at a rotation speed of 400 r / min for 1 h to obtain talc powder with a particle size of 200 mesh;

[0093] S22: Dissolve the silane coupling agent KH-570 in deionized water to prepare a silane coupling agent solution with a mass fraction of 50%. Disperse the talcum powder obtained by grinding in S21 in the silane coupling agent solution, where the mass ratio of talcum powder to silane coupling agent is 1:1, to obtain a solid-liquid mixture D;

[0094] S23: Heat the solid-liquid mixture D to 40°C, stir at a speed of 200 r / min for 2 h, then perform ultrasonic treatment for 0.5 h after stirring. After ultrasonic treatment, filter and dry at 80°C for 12 h. After drying, grind again. The speed of the ball mill is 500 r / min, and the grinding time is 2 h to obtain the modified talcum powder. The particle size of the obtained modified talcum powder is 300 mesh.

[0095] A preparation process of a super three-dimensional penetrating flower glaze. The specific process flow of the preparation process of the super three-dimensional penetrating flower glaze is as follows.

[0096] S51: Put the raw materials of glaze A into a ball mill according to the formula ratio. The speed of the ball mill is 300 r / min. After grinding for 1 h, add 40 wt% of water, 0.1 wt% of sodium carboxymethyl cellulose, and 0.4 wt% of sodium tripolyphosphate. Increase the speed of the ball mill to 500 r / min and continue grinding for 8 h. Use a magnetic iron remover to remove iron to obtain glaze A;

[0097] S52: Put the raw materials of glaze B into a ball mill according to the formula ratio. The speed of the ball mill is 300 r / min. After grinding for 1 h, add 40 wt% of water, 0.1 wt% of sodium carboxymethyl cellulose, and 0.4 wt% of sodium tripolyphosphate. Increase the speed of the ball mill to 500 r / min and continue grinding for 8 h. Use a magnetic iron remover to remove iron to obtain glaze B;

[0098] S53: Purge the surface of the green body with nitrogen. The purging flow rate of nitrogen is 8 m / s. First, pour glaze A on the surface of the green body by the glaze pouring method. The parameters of the glaze pouring method are: the glaze pouring distance is 25 cm, the specific gravity of glaze A is 1.86 g / ml, the glazing amount is 70 g / piece, the size of the brick piece is 300*600 mm. After pouring, let it stand and dry to obtain green body I;

[0099] S54: Pour glaze B on the surface of green body I by the glaze pouring method. The parameters of the glaze pouring method are: the glaze pouring distance is 25 cm, the specific gravity of glaze B is 1.86 g / ml, the glazing amount is 80 g / piece, the size of the brick piece is 300*600 mm. After pouring, put it into a drying kiln of the glaze line for drying. The temperature of the drying kiln is 200°C to obtain green body II;

[0100] S55: Print penetrating flower ink on the surface of green body II. After printing, directly put it into a kiln for firing. The temperature of the kiln is 1160°C, and the firing cycle is 65 min. After firing, cool it to room temperature to obtain a semi-finished product;

[0101] S56: The semi-finished product obtained in S55 is polished successively using the following grinding heads: a grinding head composed of 5 groups of 100-mesh hard modules, a grinding head composed of 4 groups of 600-mesh elastic modules, a grinding head composed of 4 groups of 800-mesh elastic modules, a grinding head composed of 5 groups of 1500-mesh elastic modules, and a grinding head composed of 4 groups of 2000-mesh elastic modules. The pressure exerted by the grinding head with hard abrasive blocks on the tile surface is 1.5 MPa, and the pressure exerted by the grinding heads composed of elastic modules on the tile surface is 0.5 MPa, obtaining the super three-dimensional penetrating flower glaze.

[0102] Comparative Example 1

[0103] In this comparative example, the potassium feldspar in glaze A is not modified, and the remaining steps are the same as those in Example 1.

[0104] Comparative Example 2

[0105] In this comparative example, during the modification process of potassium feldspar in glaze A, magnesium chloride and calcium nitrate are not added, and the remaining steps are the same as those in Example 1.

[0106] Comparative Example 3

[0107] In this comparative example, during the modification process of potassium feldspar in glaze A, surface modification is not carried out using boric acid solution, and the remaining steps are the same as those in Example 1.

[0108] Comparative Example 4

[0109] In this comparative example, during the modification process of potassium feldspar in glaze A, surface modification is not carried out using CTAB, and the remaining steps are the same as those in Example 1.

[0110] Comparative Example 5

[0111] In this comparative example, the talc in glaze B is not modified, and the remaining steps are the same as those in Example 1.

[0112] Comparative Example 6

[0113] In this comparative example, the potassium feldspar in glaze A is not modified, the talc in glaze B is not modified, and the remaining steps are the same as those in Example 1.

[0114] Comparative Example 7

[0115] In this comparative example, only the grinding head with hard abrasive blocks is used for grinding during the polishing process, and the remaining steps are the same as those in Example 1.

[0116] The wear resistance of the surface of the super-stereoscopic penetrating flower glaze prepared in the examples and comparative examples was tested in accordance with GB / T 3810.7-2016, the stain resistance of the surface was tested in accordance with GB / T 3810.14-2016, and the glossiness of the ceramic glaze surface was detected by a glossmeter in accordance with the GB / T 11420-2024 standard. The experimental results are summarized in the following table.

[0117] Wear resistance (level) Stain resistance (level) Glossiness (%) Example 1 5 5 95 Example 2 5 5 90 Example 3 5 5 90 Comparative Example 1 3 4 85 Comparative Example 2 4 4 80 Comparative Example 3 4 4 80 Comparative Example 4 4 4 80 Comparative Example 5 4 3 70 Comparative Example 6 3 3 70 Comparative Example 7 3 3 50

[0118] It can be seen from the experimental data that the addition of modified potassium feldspar and modified talc powder both make the prepared glaze layer have better wear resistance, stain resistance and glossiness, and the polishing treatment further improves the texture of the glaze layer.

[0119] The above are only the preferred embodiments of the present invention, and do not impose any form of limitation on the present invention. Although the present invention has been disclosed above with preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some changes or modifications to the equivalent embodiments by using the technical content disclosed above within the scope of the technical solution of the present invention. However, as long as it does not depart from the content of the technical solution of the present invention, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A super three-dimensional infiltration glaze, characterized in that: The raw materials of the infiltration glaze include glaze A and glaze B. The raw materials of glaze A are as follows: by mass percentage, modified potassium feldspar 30-35%, sodium feldspar 40-45%, kaolin 3-5%, ball clay 2-4%, quartz 5-10%, fused quartz 10-15%; Wherein, the preparation method of modified potassium feldspar is: S11: mixing potassium feldspar, magnesium chloride and calcium nitrate in a mass ratio of (3-5):1:1, and grinding the mixture in a ball mill at a speed of 400 r / min for 1 h to obtain a mixture A; S12: Dispersing the mixture A in a boric acid solution to obtain a solid-liquid mixture B with a mass fraction of 20-30%, ultrasonically treating for 0.5 h, filtering, and drying at 110° C. for 8 h to obtain a mixture C; S13: dispersing the mixture C in a 20% by mass hexadecyltrimethylammonium bromide CTAB solution, wherein the mass ratio of the mixture C to the CTAB is 1:(1-3), ultrasonicating for 0.5 h, filtering, and drying at 80° C. for 12 h. The dried mixture is heated from room temperature to 400° C. in a muffle furnace and calcined for 3 h. After calcination, the mixture is cooled and ground to a particle size of 300 meshes to obtain the modified potassium feldspar; The raw materials of glaze B are as follows, by mass percentage, potassium feldspar 30-35%, sodium feldspar 30-40%, kaolin 3-5%, ball clay 2-4%, quartz 10-15%, fused quartz 10-15%, modified talc 2-5%; Wherein, the preparation method of modified talcum powder is: S21: putting talc into a ball mill and grinding it at a speed of 400 r / min for 1 h to obtain talc powder with a particle size of 200 mesh; S22: dissolving a silane coupling agent in deionized water to obtain a silane coupling agent solution with a mass fraction of 30-50%, dispersing the talc powder obtained by grinding S21 in the silane coupling agent solution, wherein the mass ratio of the talc powder to the silane coupling agent is 1:1, to obtain a solid-liquid mixture D; S23: The solid-liquid mixture D is heated to 40°C, stirred at a speed of 150-200 r / min for 1-2 h, ultrasonicated for 0.5 h after the stirring, filtered, dried at 80°C for 12 h, and ground again after drying at a ball mill speed of 500 r / min for 2 h to obtain the modified talc powder.

2. The super three-dimensional glaze according to claim 1, characterized in that: The mass fraction of the boric acid solution in the S12 is 10-15%.

3. The super three-dimensional glaze according to claim 1, characterized in that: The heating rate of the muffle furnace in S13 is 5°C / min.

4. The super three-dimensional glaze according to claim 1, characterized in that: The modified talc powder obtained by grinding in S23 has a particle size of 300 meshes.

5. A process for preparing the super three-dimensional glaze according to any one of claims 1 to 4, characterized in that: The specific process of the preparation process of the super three-dimensional infiltration glaze is as follows: S51: putting the raw materials of glaze A into a ball mill according to the formula ratio, the speed of the ball mill is 300 r / min, after grinding for 1 hour, 40wt% of water, 0.1wt% of sodium carboxymethyl cellulose and 0.4wt% of sodium tripolyphosphate are added, the speed of the ball mill is increased to 500 r / min, and grinding is continued for 8 hours. The magnetic iron remover is used to remove iron to obtain glaze A; S52: putting the raw materials of glaze B into a ball mill according to the formula ratio, the speed of the ball mill is 300 r / min, after grinding for 1 hour, 40wt% of water, 0.1wt% of sodium carboxymethyl cellulose and 0.4wt% of sodium tripolyphosphate are added, the speed of the ball mill is increased to 500 r / min, and grinding is continued for 8 hours. The iron is removed by a magnetic iron remover to obtain glaze B; S53: nitrogen is used to purge the surface of the green body, and glaze A is first poured on the surface of the green body by a pouring method. After pouring, the green body is allowed to stand and dry to obtain body I; S54: pouring glaze B on the surface of body I by pouring glaze method, and after pouring, placing the body in a glaze line drying kiln for drying at a temperature of 200° C. to obtain body II; S55: Printing the infiltration ink on the surface of the blank II, and directly putting it into the kiln for firing after printing, the kiln temperature is 1160°C, the firing cycle is 65 minutes, and after firing, it is cooled to room temperature to obtain a semi-finished product; S56: The semi-finished product obtained in S55 is polished to obtain the super three-dimensional infiltrated glaze, and the polishing is carried out using the following grinding heads in sequence: a grinding head composed of 5 groups of 100-mesh hard modules, a grinding head composed of 4 groups of 600-mesh elastic modules, a grinding head composed of 4 groups of 800-mesh elastic modules, a grinding head composed of 5 groups of 1500-mesh elastic modules and a grinding head composed of 4 groups of 2000-mesh elastic modules; the pressure applied by the grinding head of the polishing hard grinding block on the surface of the tile is 1.5 MPa, and the pressure applied by the grinding head composed of the elastic modules on the surface of the tile is 0.3-0.5 MPa.

6. The process for preparing a super three-dimensional infiltrated glaze according to claim 5, characterized in that: The purge flow rate of nitrogen in S53 is 8 m / s.

7. The process for preparing a super three-dimensional glaze according to claim 5, characterized in that: The parameters of the glazing method in S53 are: glazing distance 25 cm, specific gravity of glaze A 1.83~1.86g / ml, glazing amount 70g / piece, and tile size 300*600mm.

8. The process for preparing a super three-dimensional glaze according to claim 5, characterized in that: The parameters of the glazing method in S54 are: glazing distance 25 cm, specific gravity of glaze B 1.83~1.86g / ml, glazing amount 80g / piece, and tile size 300*600mm.

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