Digital glaze, preparation method of digital glaze, fine matte super-wear-resistant marble tile and preparation method of fine matte super-wear-resistant marble tile

Abstract

The invention relates to the technical field of ceramic tile glaze, in particular to digital glaze and a preparation method thereof, and a fine matte super-wear-resistant marble ceramic tile and a preparation method thereof. The invention discloses digital glaze which comprises the following raw materials in parts by weight: 35-45 parts of digital powder, 35-55 parts of a solvent, 5-12 parts of a dispersing agent and 5-12 parts of an auxiliary agent, every 100 parts of digital powder comprises the following raw materials in parts by weight: 35 parts of potassium feldspar, 17 parts of modified quartz, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, 3 parts of zinc oxide and 10 parts of wear-resistant frit. The digital glaze has the advantages of being good in color development, fine and smooth in hand feeling, free of pinhole miliaria and good in wear resistance, and the quality of marble tile products is greatly improved.

Description

Technical Field

[0001] The invention relates to the technical field of tile glazes, and in particular to digital glaze and a preparation method thereof, and fine matte super wear-resistant marble tiles and a preparation method thereof. Background Art

[0002] In the ceramic industry, the glazes used in the traditional bell-shaped glazing and spray gun glazing processes are pure water glazes. After glazing, they will seriously affect the body strength of large-sized ultra-thin marble tile products, causing them to crack easily during the firing process or break easily during later processing.

[0003] As a solid-liquid mixture, digital glaze replaces colorants, printing oils, printing glazes and other additives. Its advantage is that it can increase the richness of patterns and improve clarity. At the same time, it can be adjusted according to different kiln temperatures, different feel, glossiness, and transparency. Its processing process, solvent materials, application performance, etc. are very close to ink, and can be printed on the surface of tiles through inkjet nozzles. It not only saves the amount of glaze, but also makes the glaze thickness uniform. In addition, digital glaze is an oily or low-oily substance with a low water content, which reduces the impact on the strength of the brick blank, and will not produce defects such as glaze marks during sintering.

[0004] However, the current ceramic digital glaze still has defects such as poor color, insufficient glaze feel, pinholes and rashes on the glaze, and poor wear resistance.

[0005] To this end, the present application provides digital glaze and a preparation method thereof, delicate matte super wear-resistant marble tiles and a preparation method thereof. Summary of the invention

[0006] The present application provides digital glaze and a preparation method thereof, fine matte ultra-wear-resistant marble tiles and a preparation method thereof. The digital glaze has the advantages of good color, fine hand feel, no pinholes and prickly heat, and good wear resistance, which greatly improves the quality of marble tile products.

[0007] The technical solution adopted by this application to solve its technical problem is:

[0008] In a first aspect, the present application provides a digital glaze, comprising the following raw materials in parts by weight:

[0009] 35-45 parts of digital powder, 35-55 parts of solvent, 5-12 parts of dispersant, 5-12 parts of additives;

[0010] Every 100 parts of digital powder includes the following raw materials in parts by weight:

[0011] 35 parts of potassium feldspar, 17 parts of modified quartz, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, 3 parts of zinc oxide, 10 parts of wear-resistant frit;

[0012] Every 100 parts of modified quartz includes the following raw materials in parts by weight:

[0013] 7 parts of titanium dioxide, 78 parts of quartz sand, 15 parts of color frit;

[0014] The preparation process of modified quartz is as follows: preparing materials according to the weight composition of 100 parts of modified quartz; adding titanium dioxide and coloring frit into quartz sand, fully mixing, ball milling and sintering, the sintering temperature is 1300-1320°C, and the modified quartz is obtained after the sintering is completed.

[0015] In some embodiments, the solvent is di(2-ethylhexyl) adipate.

[0016] In some embodiments, the dispersant includes polyethylene wax and polyvinyl pyrrolidone.

[0017] In some embodiments, the auxiliary agent is polyoxyethylene stearate.

[0018] In some embodiments, the chemical composition of the wear-resistant frit is:

[0019] CaO: 10.28%, SiO2: 50.06%, Fe2O3: 0.11%, MgO: 3.87%, TiO2: 0.06%, Al2O3: 20.92%, K2O: 0. 23%, Na2O: 2.55%, ZnO: 1%, BaO: 6.71%, SrO: 4.08%, ZrO2: 0.01%, B2O3: 0.03%, Loss: 0.09%.

[0020] In some embodiments, the chemical composition of the chromonic frit is:

[0021] CaO: 12.7%, SiO2: 63.47%, Fe2O3: 0.35%, MgO: 1.78%, TiO2: 0.11%, Al2O3: 8.3%, K2O: 4.44%, Na2O: 1.29 %, ZnO: 3.4%, BaO: 2.28%, ZrO2: 0.31%, B2O3: 0.97%, PbO: 0.08%, P2O3: 0.29%, Li2O: 0.02%, Loss: 0.21%.

[0022] In some embodiments, the weight ratio of polyethylene wax to polyvinyl pyrrolidone in the dispersant is 2:(1-3).

[0023] In a second aspect, the present application provides a method for preparing the digital glaze, comprising the following steps:

[0024] Prepare the materials according to the weight composition of the digital powder;

[0025] Each single raw material of the digital powder is wet ball-milled to a D99 of less than 5 μm, and then dried;

[0026] Prepare corresponding digital powder by mixing according to weight parts;

[0027] Mix the dispersant, additives and part of the solvent and stir evenly, add the digital powder and ball mill until the D90 reaches 1.0-1.2μm, then add the remaining solvent;

[0028] Filter to obtain digital glaze.

[0029] In a third aspect, the present application provides delicate matte super wear-resistant marble tiles, characterized in that they include the digital glaze described above.

[0030] In a fourth aspect, the present application provides a method for preparing the fine matte ultra-wear-resistant marble tile, comprising the following steps:

[0031] Preparation of digital glaze;

[0032] Pour the glaze on the body, print the pattern by inkjet, and then print the digital glaze by inkjet;

[0033] After high-temperature firing in a kiln, fine matte and ultra-wear-resistant marble tiles are obtained.

[0034] The beneficial effects of this application are:

[0035] 1. The digital glaze described in this application is designed to solve the problem that large-sized ultra-thin marble tile products cannot use traditional glazing processes (such as bell-shaped glazing and spray gun glazing). A digital glaze that can use a full digital glazing process and its preparation method have been developed, breaking the monopoly of foreign technology.

[0036] 2. Existing digital glazes on the market are prone to defects such as poor color, rough and unsophisticated glaze surface, and pinholes and prickly heat on the glaze surface, and poor wear resistance. In response to the above problems, the digital glaze described in this application increases the aluminum content of the digital powder to improve the wear resistance of the glaze layer, adds modified quartz to promote color development, and adds wear-resistant frit to improve the color development of the digital glaze and increase its use temperature range. A digital glaze with good color development, delicate hand feel, no pinholes and prickly heat, and high wear resistance is prepared, which greatly improves the quality and grade of marble tile products.

[0037] 3. The digital glaze preparation method of the present application has better compatibility and is less likely to drip ink after multi-stage filtration. At the same time, it ensures that the particles in the final product obtained through filtration are within the standard range, will not clog the filter of the inkjet printer, and has a longer storage time. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] The present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0039] Figure 1 This is a process flow chart of the preparation method of the digital glaze described in this application. DETAILED DESCRIPTION

[0040] In order to facilitate the understanding of those skilled in the art, the present invention is further described below in conjunction with embodiments, and the contents mentioned in the implementation modes are not intended to limit the present invention.

[0041] As used herein, "and / or" includes the term of any and all combinations of one or more associated listed items. The terms used herein are only used to describe specific embodiments and are not intended to limit the present invention. As used herein, the singular forms "a", "an", "an" and "the" are also intended to include the plural forms, unless the context clearly indicates otherwise. It is further understood that "including", when used in this specification, specifies the stated features, integers, steps, operations, elements and / or compositions, but does not exclude the existence or addition of one or more other features, integers, steps, operations, elements, compositions and / or combinations thereof.

[0042] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the invention belongs. It is further understood that terms, such as defined in commonly used dictionaries, are interpreted in accordance with their meanings in the context of the relevant art and are not in an idealized or overly formal sense unless explicitly so defined herein.

[0043] The exemplary invention described herein may appropriately lack any one or more element limitations that are not specifically disclosed herein. Therefore, the terms "comprise", "include", "contain", etc. should be understood broadly and non-restrictively. In addition, the terminology used herein is used as a description, not a limitation, and it is unintentional to use these terminology expressions that do not include any equivalent characteristics, but only describe some of their characteristics, but various modifications are possible within the scope of the present invention according to the rights. Therefore, although the present invention has been specifically disclosed by preferred embodiments and optional features, the modifications disclosed herein to embody the changes of the present invention may be recorded by those skilled in the art, and such modifications and changes will be considered to be within the scope of the present invention.

[0044] Terminology explanation:

[0045] Ball milling is a material processing technology that crushes and mixes materials through grinding media (such as steel balls, ceramic balls, etc.) in a rotating or vibrating cylinder. In the preparation process of ceramic glazes, ball milling is usually used to refine the raw materials to the required particle size range to increase the uniformity and activity of the raw materials and promote subsequent chemical reactions and physical mixing. In the preparation process of the digital glaze of this application, each single raw material of the digital powder needs to be wet-milled to ensure that its fineness reaches D99 < 5μm, thereby improving the performance and stability of the glaze.

[0046] Green body refers to the semi-finished product that has not been sintered after the pressing and molding process in the production process of ceramic products. Green body is usually made of ceramic raw materials (such as clay, quartz, feldspar, etc.) through mixing, molding (such as pressing, grouting, etc.). In the production of ceramic tiles, green body is the basis of the final product, on which various glazes will be applied and sintered to obtain finished ceramic tiles with decorative and usable performance.

[0047] The top glaze is a layer of glaze applied to the surface of the ceramic body, which mainly plays a decorative and protective role. The top glaze can give the ceramic products rich colors, gloss and texture, and at the same time can resist the damage of external factors such as wear and corrosion, and extend the service life of the ceramic products. In this application, the preparation method of the fine matte super wear-resistant marble tile firstly pours the top glaze on the body, and then inkjet prints the pattern and digital glaze to form the final decorative effect.

[0048] Inkjet printing patterns is a technology that uses an inkjet printer to print patterns directly on a ceramic body or glaze. In tile production, inkjet printing technology can achieve highly personalized pattern design and color expression, and increase the added value of the product. The process of inkjet printing patterns usually involves accurately spraying pigmented ink onto a body or glaze through a nozzle to form fine patterns and color levels. In this application, the method for preparing fine matte and ultra-wear-resistant marble tiles, the inkjet printing pattern is the next process after being applied on the glaze, which is used to further beautify the appearance of the tile.

[0049] In view of the problems that the existing digital glazes on the market are prone to color difference, rough and not fine glaze surface, pinholes and prickly heat on the glaze surface, and poor wear resistance, the present application provides a digital glaze, including the following raw materials in parts by weight:

[0050] 35-45 parts of digital powder, 35-55 parts of solvent, 5-12 parts of dispersant, 5-12 parts of additives;

[0051] Every 100 parts of digital powder includes the following raw materials in parts by weight:

[0052] 35 parts of potassium feldspar, 17 parts of modified quartz, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, 3 parts of zinc oxide, 10 parts of wear-resistant frit;

[0053] Every 100 parts of modified quartz includes the following raw materials in parts by weight:

[0054] 7 parts of titanium dioxide, 78 parts of quartz sand, 15 parts of color frit;

[0055] The preparation process of modified quartz is as follows: preparing materials according to the weight composition of 100 parts of modified quartz; adding titanium dioxide and coloring frit into quartz sand, fully mixing, ball milling and sintering, the sintering temperature is 1300-1320°C, and the modified quartz is obtained after the sintering is completed.

[0056] It can be understood that digital powder is the main material that constitutes digital glaze, which includes potassium feldspar, modified quartz, dolomite, corundum and other minerals and compounds. These raw materials are formed into powders with specific chemical composition and physical properties through specific proportions and processing, providing digital glaze with the required color, glossiness, wear resistance and other basic properties; specifically, potassium feldspar and dolomite can be used as flux to reduce the melting temperature of the glaze; corundum, calcined alumina, etc. improve the hardness and wear resistance of the glaze layer; modified quartz enhances the coloring ability and glossiness of the glaze through its special chemical composition and physical properties.

[0057] In the present application, the weight of digital powder is 35-45 parts (including endpoint values), for example, it can be 35 parts, 37 parts, 40 parts, 41 parts. The appropriate weight of digital powder can ensure the fluidity, stability and sintering performance of the glaze, so as to obtain a uniform, dense and wear-resistant glaze layer; if the digital powder is too much, the glaze will be too thick, the fluidity will be poor, and it will be difficult to glaze evenly; at the same time, too much powder will also increase the thickness of the glaze layer and the difficulty of sintering, which may easily cause the glaze surface to crack or bubble. On the contrary, if the digital powder is too little, the glaze layer will be too thin, it will be difficult to form a stable glaze surface, and the color, glossiness and wear resistance will be affected.

[0058] Specifically, the titanium dioxide and coloring agent in the modified quartz react chemically with quartz sand at high temperature to form stable compounds, which form a dense structure in the glaze layer, improving the hardness and wear resistance of the glaze. At the same time, the coloring frit in the modified quartz can also promote the uniform distribution and brightness of the glaze color, so that the tiles have a better decorative effect. The prepared modified quartz can improve the wear resistance, chemical corrosion resistance and coloring effect of the glaze.

[0059] Specifically, the preparation process of the modified quartz is as follows: according to the weight parts of 100 parts of the modified quartz, corresponding weight parts of quartz sand, titanium dioxide, and color frit are weighed; titanium dioxide and color frit are added to the quartz sand, and the mixture is fully mixed and then ball milled. The ball milling time is 2-3 hours, and sintering is performed. The sintering temperature is controlled at 1300-1320° C., and the sintering time is controlled at 0.8-1.2 hours. After the sintering is completed, the modified quartz is obtained;

[0060] In some embodiments, the solvent is diisooctyl adipate. The solvent mainly improves the stability of the ink, making its viscosity, surface tension, etc. less likely to change with temperature. The choice of solvent has an important influence on the fluidity, drying speed, sintering performance, etc. of the glaze. Diisooctyl adipate has good solubility and volatility, and can effectively disperse the digital powder evenly during the preparation process to form a stable suspension. At the same time, the volatility of the solvent also affects the drying speed and sintering performance of the glaze, thereby affecting the final quality of the tile.

[0061] In the present application, the weight of the solvent is 35-55 parts (including the endpoint values), for example, it can be 35 parts, 37 parts, 40 parts, 45 parts, 48 ​​parts, 55 parts, and the appropriate solvent content can ensure the uniformity and stability of the glaze, while controlling the thickness and sintering performance of the glaze layer. Too much solvent will make the glaze too thin, resulting in insufficient glaze thickness, affecting the color, gloss and wear resistance of the tile; at the same time, too much solvent will also increase the drying time and energy consumption during the sintering process. If the solvent is too little, the glaze is too thick, it is difficult to glaze evenly, and it is easy to produce defects such as pinholes and bubbles.

[0062] In some embodiments, the dispersant includes polyethylene wax and polyvinyl pyrrolidone. The dispersant is mainly used to prevent the digital powder from agglomerating and precipitating in the solvent, and to maintain the uniformity and stability of the glaze. Dispersants such as polyethylene wax and polyvinyl pyrrolidone are adsorbed on the surface of digital powder particles through their unique molecular structure and surface properties to form a protective film to prevent direct contact and agglomeration between particles. In the present application, the weight of the dispersant is 5-12 parts (including endpoint values), for example, it can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 12 parts, and the right amount of dispersant can maintain the uniformity and stability of the glaze, while preventing agglomeration and precipitation between particles. Too much dispersant may cause the glaze to be too viscous and affect fluidity; at the same time, too much dispersant may also affect the sintering performance and final quality of the glaze. If the dispersant is too little, the agglomeration and precipitation of the digital powder cannot be effectively prevented, resulting in uneven and unstable glaze.

[0063] Specifically, the weight ratio of polyethylene wax to polyvinyl pyrrolidone in the dispersant is 2:(1-3). A suitable ratio of polyethylene wax to polyvinyl pyrrolidone helps to improve the dispersion effect.

[0064] In some embodiments, the auxiliary agent is stearic acid polyoxyethylene ether. The auxiliary agent has good emulsification and thickening properties, can increase the interaction between powder particles and solvent, and make the glaze system more stable.

[0065] In the present application, the weight of the additive is 5-12 parts (including the endpoint values), for example, it can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 12 parts. The right amount of additive can increase the interaction between the powder particles and the solvent, making the glaze system more stable. Too much additive may cause the glaze to be too viscous and affect fluidity; if the additive is too little, it will not be able to effectively prevent the aggregation and precipitation of the digital powder, resulting in uneven and unstable glaze.

[0066] In some embodiments, the chemical composition of the wear-resistant frit is:

[0067] CaO: 10.28%, SiO2: 50.06%, Fe2O3: 0.11%, MgO: 3.87%, TiO2: 0.06%, Al2O3: 20.92%, K2O: 0.23%, Na2O: 2.55%, ZnO: 1%, BaO: 6.71%, SrO: 4.08%, ZrO2: 0.01%, B2O3: 0.03%, Loss: 0.09%. The wear-resistant frit contains high-hardness oxides such as alumina (Al2O3) and a variety of wear-resistant components, which can form a high-hardness glaze layer during the sintering process, thereby significantly improving the wear resistance of the tile surface; the wear-resistant frit with a specific chemical composition has good thermal stability, chemical corrosion resistance, high wear resistance and high hardness, and can also improve the coloring effect of the inkjet pattern.

[0068] In some embodiments, the chemical composition of the chromonic frit is:

[0069] CaO: 12.7%, SiO2: 63.47%, Fe2O3: 0.35%, MgO: 1.78%, TiO2: 0.11%, Al2O3: 8.3%, K2O: 4.44%, Na2O: 1.29 %, ZnO: 3.4%, BaO: 2.28%, ZrO2: 0.31%, B2O3: 0.97%, PbO: 0.08%, P2O3: 0.29%, Li2O: 0.02%, Loss: 0.21%.

[0070] The color-producing frit has a strong luster, high transparency, and a strong fluxing effect. It can form a glass phase during the sintering process, improve the transparency and gloss of the glaze, and promote the uniform distribution and brightness of the glaze color.

[0071] The method for preparing the digital glaze described above comprises the following steps:

[0072] Each raw material of the digital powder is wet ball milled to process each raw material to D99<5μm, and then sieved (through a 325 mesh screen) and dried (the water content of each powder is less than 0.1%).

[0073] Prepare corresponding digital powder by mixing according to weight parts;

[0074] Mix the dispersant, additives and part of the solvent and stir evenly, add the digital powder and ball mill until the D90 reaches 1.0-1.2μm, then add the remaining solvent;

[0075] Filter to obtain digital glaze.

[0076] The specific process is as follows: S1, wet ball milling each single raw material in the digital powder to process each raw material to D99<5μm, and sieving them respectively after processing;

[0077] S2, drying the powders sieved in step S1;

[0078] S3, adding the powders dried in step S2 into a high-speed mixer according to the proportion of digital powders to obtain digital powders;

[0079] S4, mixing the dispersant, the additive and part of the solvent evenly, and then adding them into the sand mill and continuing to stir;

[0080] S5, slowly add the digital powder processed in step S3 to the sand mill, grind repeatedly until the protective glaze powder is processed to a D90 of 1.0-1.2 μm, and then add the remaining solvent (the mass ratio of the partial solvent to the remaining solvent is 7-8: (2-3)) to adjust the viscosity and density of the system;

[0081] S6. Filter the mixture obtained in step S5 through a filter hole to obtain digital glaze.

[0082] In the step S1, the ball milling treatment time is 2-3 hours, and each of the powders after the ball milling treatment is passed through a 325-mesh sieve;

[0083] In step S2, the drying temperature is 120-140° C., and the moisture content of each of the powders after drying is less than 0.1%;

[0084] In step S3, the mixing time of each powder in the high-speed mixer is 20-30 minutes, and the rotation speed is 100-150 rpm;

[0085] In the step S5, the sand grinding time of each of the powders in the sand mill is 2-10 hours. After sand grinding, the D90 of each of the powders reaches 1.0-1.2 um.

[0086] In the step S5, the digital glaze ink is filtered through filter membranes with pore diameters of 10 μm, 5 μm, 3 μm, and 1 μm in sequence, and the filtrate finally obtained is the digital glaze ink for full digital spray glazing.

[0087] The preparation method of fine matte ultra-wear-resistant marble tiles comprises the following steps:

[0088] Preparation of digital glaze;

[0089] Pour the glaze on the body, print the pattern by inkjet, and then print the digital glaze by inkjet;

[0090] After high-temperature firing in a kiln, fine matte and ultra-wear-resistant marble tiles are obtained.

[0091] Specifically, the preparation process of digital glazed ceramic tiles with a specification of 1600mm×3200mm is as follows: use conventional ceramic blanks to press into blanks → pour conventional glaze on the blanks → inkjet print patterns → inkjet print digital glaze → after high-temperature firing in a kiln, marble tiles are obtained.

[0092] More specifically, pour conventional glaze on the body, select the appropriate glaze formula (common glaze), the viscosity, fluidity and drying speed of the glaze need to match the characteristics of the body; use automated glazing equipment to evenly pour the glaze on the body surface to ensure that the entire surface is covered with glaze and the thickness is consistent. After pouring the glaze, the body needs to be pre-dried to remove the moisture in the glaze and form a uniform glaze surface;

[0093] The process of inkjet printing patterns is as follows: according to the design requirements, use professional inkjet printing equipment to print the pattern directly on the dried glaze. After printing, perform appropriate curing or drying treatment;

[0094] Inkjet printing digital glaze, the process is: according to the different requirements of tile surface gloss and feel, choose single-channel or dual-channel inkjet printing, the channel grayscale is generally between 30-90% for inkjet printing digital glaze;

[0095] The process of high-temperature firing in a kiln is as follows: the tiles with printed digital glaze are sent into the kiln and fired at 1170-1220℃ for 50-60 minutes.

[0096] Preparation Example 1

[0097] 100 parts of modified quartz, including the following raw materials in parts by weight:

[0098] 7 parts of titanium dioxide, 78 parts of quartz sand, 15 parts of color frit;

[0099] The preparation process of modified quartz is as follows: preparing materials according to the weight composition of 100 parts of modified quartz; adding titanium dioxide and coloring frit into quartz sand, fully mixing, ball milling, and sintering; the sintering temperature is controlled at 1300-1320° C., the sintering time is controlled at 0.8-1.2 hours, and the modified quartz is obtained after the sintering;

[0100] The chemical composition of the chromogenic frit is:

[0101] CaO: 12.7%, SiO2: 63.47%, Fe2O3: 0.35%, MgO: 1.78%, TiO2: 0.11%, Al2O3: 8.3%, K2O: 4.44%, Na2O: 1.29 %, ZnO: 3.4%, BaO: 2.28%, ZrO2: 0.31%, B2O3: 0.97%, PbO: 0.08%, P2O3: 0.29%, Li2O: 0.02%, Loss: 0.21%.

[0102] Preparation Example 2

[0103] Every 100 parts of digital powder includes the following raw materials in parts by weight:

[0104] 35 parts of potassium feldspar, 17 parts of modified quartz (Preparation Example 1), 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, 3 parts of zinc oxide, and 10 parts of wear-resistant frit;

[0105] The preparation method of digital powder comprises the following steps:

[0106] Each raw material of the digital powder is wet ball milled to process each raw material to D99<5μm, and then sieved (through a 325-mesh sieve) and dried (the water content of each powder is less than 0.1%).

[0107] According to the weight composition of 100 parts of digital powder, weigh the dried powder: 35 parts of potassium feldspar, 17 parts of modified quartz, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, 3 parts of zinc oxide, and 10 parts of wear-resistant frit, add them into a high-speed mixer for mixing (for example, the mixing time is 30 minutes and the speed is 150 rpm) to obtain digital powder.

[0108] Example 1

[0109] Digital glaze comprises the following raw materials in parts by weight:

[0110] 35 parts of digital powder (Preparation Example 2), 35 parts of diethylhexyl adipate, 5 parts of polyethylene wax and polyvinyl pyrrolidone, and 5 parts of stearic acid polyoxyethylene ether;

[0111] The preparation method of digital glaze comprises the following steps:

[0112] S1. According to the weight composition of the above digital glaze, weigh the corresponding raw materials;

[0113] S2. The dispersant, additive and part of the solvent are mixed and stirred evenly and then added to the sand mill and continued to stir;

[0114] S3. Slowly add the digital powder to the sand mill, grind repeatedly until the digital powder is processed to a D90 of 1.0-1.2 μm, then add the remaining solvent, mix thoroughly, and obtain a mixed liquid;

[0115] S4. The mixed liquid obtained in step S3 is filtered through filter membranes with pore diameters of 10 μm, 5 μm, 3 μm, and 1 μm in sequence, and the filtrate obtained after filtration is the digital glaze.

[0116] Example 2

[0117] Digital glaze comprises the following raw materials in parts by weight:

[0118] 45 parts of digital powder (Preparation Example 2), 55 parts of diethylhexyl adipate, 12 parts of polyethylene wax and polyvinyl pyrrolidone, and 12 parts of stearic acid polyoxyethylene ether;

[0119] The preparation method of digital glaze comprises the following steps:

[0120] S1. According to the weight composition of the above digital glaze, weigh the corresponding raw materials;

[0121] S2. The dispersant, additive and part of the solvent are mixed and stirred evenly and then added to the sand mill and continued to stir;

[0122] S3. Slowly add the digital powder to the sand mill, grind repeatedly until the digital powder is processed to a D90 of 1.0-1.2 μm, then add the remaining solvent, mix thoroughly, and obtain a mixed liquid;

[0123] S4. The mixed liquid obtained in step S3 is filtered through filter membranes with pore diameters of 10 μm, 5 μm, 3 μm, and 1 μm in sequence, and the filtrate obtained after filtration is the digital glaze.

[0124] Example 3

[0125] Digital glaze comprises the following raw materials in parts by weight:

[0126] 40 parts of digital powder (Preparation Example 2), 40 parts of diethylhexyl adipate, 8 parts of polyethylene wax and polyvinyl pyrrolidone, and 8 parts of stearic acid polyoxyethylene ether;

[0127] The preparation method of digital glaze comprises the following steps:

[0128] S1. According to the weight composition of the above digital glaze, weigh the corresponding raw materials;

[0129] S2. The dispersant, additive and part of the solvent are mixed and stirred evenly and then added to the sand mill and continued to stir;

[0130] S3. Slowly add the digital powder to the sand mill, grind repeatedly until the digital powder is processed to a D90 of 1.0-1.2 μm, then add the remaining solvent, mix thoroughly, and obtain a mixed liquid;

[0131] S4. The mixed liquid obtained in step S3 is filtered through filter membranes with pore diameters of 10 μm, 5 μm, 3 μm, and 1 μm in sequence, and the filtrate obtained after filtration is the digital glaze.

[0132] Example 4

[0133] Digital glaze comprises the following raw materials in parts by weight:

[0134] 40 parts of digital powder (Preparation Example 2), 50 parts of diethylhexyl adipate, 10 parts of polyethylene wax and polyvinyl pyrrolidone, and 10 parts of stearic acid polyoxyethylene ether;

[0135] The preparation method of digital glaze comprises the following steps:

[0136] S1. According to the weight composition of the above digital glaze, weigh the corresponding raw materials;

[0137] S2. The dispersant, additive and part of the solvent are mixed and stirred evenly and then added to the sand mill and continued to stir;

[0138] S3. Slowly add the digital powder to the sand mill, grind repeatedly until the digital powder is processed to a D90 of 1.0-1.2 μm, then add the remaining solvent, mix thoroughly, and obtain a mixed liquid;

[0139] S4. The mixed liquid obtained in step S3 is filtered through filter membranes with pore diameters of 10 μm, 5 μm, 3 μm, and 1 μm in sequence, and the filtrate obtained after filtration is the digital glaze.

[0140] Example 5

[0141] Digital glaze comprises the following raw materials in parts by weight:

[0142] 37 parts of digital powder (Preparation Example 2), 38 parts of diethylhexyl adipate, 9 parts of polyethylene wax and polyvinyl pyrrolidone, and 9 parts of stearic acid polyoxyethylene ether;

[0143] The preparation method of digital glaze comprises the following steps:

[0144] S1. According to the weight composition of the above digital glaze, weigh the corresponding raw materials;

[0145] S2. The dispersant, additive and part of the solvent are mixed and stirred evenly and then added to the sand mill and continued to stir;

[0146] S3. Slowly add the digital powder to the sand mill, grind repeatedly until the digital powder is processed to a D90 of 1.0-1.2 μm, then add the remaining solvent, mix thoroughly, and obtain a mixed liquid;

[0147] S4. The mixed liquid obtained in step S3 is filtered through filter membranes with pore diameters of 10 μm, 5 μm, 3 μm, and 1 μm in sequence, and the filtrate obtained after filtration is the digital glaze.

[0148] Example 6

[0149] The preparation method of fine matte ultra-wear-resistant marble tiles comprises the following steps:

[0150] Use conventional ceramic blanks to press into blanks → pour conventional glaze on the blanks → inkjet print patterns → inkjet print digital glaze (Example 1) → after high-temperature firing in a kiln, ceramic tiles are obtained.

[0151] Among them, for inkjet printing digital glaze, dual-channel inkjet printing is selected, and the grayscale of both channels is 50% to perform inkjet printing digital glaze;

[0152] The process of high-temperature firing in a kiln is as follows: the tiles with printed digital glaze are sent into the kiln and fired at 1220°C for a period of 50 minutes.

[0153] Example 7

[0154] The preparation method of fine matte ultra-wear-resistant marble tiles comprises the following steps:

[0155] Use conventional ceramic blanks to press into blanks → pour conventional glaze on the blanks → inkjet print patterns → inkjet print digital glaze (Example 2) → after high-temperature firing in a kiln, ceramic tiles are obtained.

[0156] Example 8

[0157] The preparation method of fine matte ultra-wear-resistant marble tiles comprises the following steps:

[0158] Use conventional ceramic blanks to press into blanks → pour conventional glaze on the blanks → inkjet print patterns → inkjet print digital glaze (Example 3) → after high-temperature firing in a kiln, ceramic tiles are obtained.

[0159] Example 9

[0160] The preparation method of fine matte ultra-wear-resistant marble tiles comprises the following steps:

[0161] Use conventional ceramic blanks to press into blanks → pour conventional glaze on the blanks → inkjet print patterns → inkjet print digital glaze (Example 4) → after high-temperature firing in a kiln, ceramic tiles are obtained.

[0162] Example 10

[0163] The preparation method of fine matte ultra-wear-resistant marble tiles comprises the following steps:

[0164] Use conventional ceramic blanks to press into blanks → pour conventional glaze on the blanks → inkjet print patterns → inkjet print digital glaze (Example 5) → after high-temperature firing in a kiln, ceramic tiles are obtained.

[0165] Comparative Example 1

[0166] The method for preparing marble tiles comprises the following steps:

[0167] Use conventional ceramic blanks to press into blanks → pour conventional glaze on the blanks → inkjet print patterns → sinter at high temperature in a kiln to obtain ceramic tiles.

[0168] The tiles are fired at high temperature in a kiln. The process is as follows: the tiles with printed digital glaze are sent into the kiln and fired at 1220°C for 50 minutes.

[0169] Comparative Example 2

[0170] Every 100 parts of digital powder includes the following raw materials in parts by weight:

[0171] 35 parts of potassium feldspar, 17 parts of quartz sand, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, 3 parts of zinc oxide, 10 parts of wear-resistant frit;

[0172] The preparation method of digital powder comprises the following steps:

[0173] Each raw material of the digital powder is wet ball milled to process each raw material to D99<5μm, and then sieved (through a 325-mesh sieve) and dried (the water content of each powder is less than 0.1%).

[0174] According to the weight composition of 100 parts of digital powder, weigh the dried powder: 35 parts of potassium feldspar, 17 parts of quartz sand, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, 3 parts of zinc oxide, and 10 parts of wear-resistant frit, add them into a high-speed mixer for mixing (for example, the mixing time is 30 minutes and the speed is 150 rpm) to obtain digital powder.

[0175] Digital glaze comprises the following raw materials in parts by weight:

[0176] 35 parts of digital powder, 35 parts of diethyl hexyl adipate, 5 parts of polyethylene wax and polyvinyl pyrrolidone, 5 parts of stearic acid polyoxyethylene ether; the specific preparation method is consistent with Example 1;

[0177] The specific preparation method of the marble tile and the digital glaze is the same as that of Example 6;

[0178] Comparative Example 3

[0179] 100 parts of modified quartz, including the following raw materials in parts by weight:

[0180] 7 parts of titanium dioxide, 93 parts of quartz sand;

[0181] The preparation process of modified quartz is as follows: preparing materials according to the weight composition of 100 parts of modified quartz; adding titanium dioxide to quartz sand, ball milling and sintering after fully mixing, the sintering temperature is controlled at 1300-1320° C., the sintering time is controlled at 0.8-1.2 hours, and the modified quartz is obtained after the sintering is completed;

[0182] Every 100 parts of digital powder includes the following raw materials in parts by weight:

[0183] 35 parts of potassium feldspar, 17 parts of modified quartz, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, 3 parts of zinc oxide, 10 parts of wear-resistant frit;

[0184] The preparation method of digital powder comprises the following steps:

[0185] Each raw material of the digital powder is wet ball milled to process each raw material to D99<5μm, and then sieved (through a 325-mesh sieve) and dried (the water content of each powder is less than 0.1%).

[0186] According to the weight composition of 100 parts of digital powder, weigh the dried powder: 35 parts of potassium feldspar, 17 parts of modified quartz, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, 3 parts of zinc oxide, and 10 parts of wear-resistant frit, add them into a high-speed mixer for mixing (for example, the mixing time is 30 minutes and the speed is 150 rpm) to obtain digital powder.

[0187] Digital glaze comprises the following raw materials in parts by weight:

[0188] 35 parts of digital powder (Preparation Example 2), 35 parts of diisooctyl adipate, 5 parts of polyethylene wax and polyvinyl pyrrolidone, and 5 parts of stearic acid polyoxyethylene ether; the specific preparation method of digital glaze is consistent with that of Example 1;

[0189] Marble tiles, the specific preparation method is consistent with Example 6;

[0190] Comparative Example 4

[0191] 100 parts of modified quartz, including the following raw materials in parts by weight:

[0192] 7 parts of titanium dioxide, 78 parts of quartz sand, 15 parts of color frit;

[0193] The preparation process of modified quartz is as follows: preparing materials according to the weight composition of 100 parts of modified quartz; adding titanium dioxide and coloring frit into quartz sand, fully mixing, ball milling, and sintering; the sintering temperature is controlled at 1300-1320° C., the sintering time is controlled at 0.8-1.2 hours, and the modified quartz is obtained after the sintering;

[0194] The chemical composition of the chromogenic frit is:

[0195] CaO: 12.7%, SiO2: 63.47%, Fe2O3: 0.35%, MgO: 1.78%, TiO2: 0.11%, Al2O3: 8.3%, K2O: 4.44%, Na2O: 1.29 %, ZnO: 3.4%, BaO: 2.28%, ZrO2: 0.31%, B2O3: 0.97%, PbO: 0.08%, P2O3: 0.29%, Li2O: 0.02%, Loss: 0.21%.

[0196] Every 100 parts of digital powder includes the following raw materials in parts by weight:

[0197] 45 parts of potassium feldspar, 17 parts of modified quartz, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, and 3 parts of zinc oxide;

[0198] The preparation method of digital powder comprises the following steps:

[0199] Each raw material of the digital powder is wet ball milled to process each raw material to D99<5μm, and then sieved (through a 325-mesh sieve) and dried (the water content of each powder is less than 0.1%).

[0200] According to the weight composition of 100 parts of digital powder, weigh the dried powder: 45 parts of potassium feldspar, 17 parts of modified quartz, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, and 3 parts of zinc oxide, add them into a high-speed mixer for mixing (for example, the mixing time is 30 minutes and the speed is 150 rpm) to obtain digital powder.

[0201] Digital glaze comprises the following raw materials in parts by weight:

[0202] 35 parts of digital powder (Preparation Example 2), 35 parts of diisooctyl adipate, 5 parts of polyethylene wax and polyvinyl pyrrolidone, and 5 parts of stearic acid polyoxyethylene ether; the specific preparation method of digital glaze is consistent with that of Example 1;

[0203] Marble tiles, the specific preparation method is consistent with Example 6;

[0204] The marble tiles prepared in the above examples and comparative examples were tested for the following performance items, and the test results are summarized in the following Table 1:

[0205] Hair color: Use a color card to compare hair color;

[0206] Pinholes and prickly heat are expressed by counting the number;

[0207] Wear resistance: the wear resistance of imitation marble tiles is tested according to GBT3810.7-2016, the test standard for the determination of the wear resistance of glazed tile surfaces;

[0208] Table 1

[0209] Color ability Number of pinholes Number of prickly heat Wear resistance grade Example 6 Excellent none none 5 Example 7 Excellent none none 5 Example 8 Excellent none none 5 Example 9 Excellent none none 5 Example 10 Excellent none none 5 Comparative Example 1 Poor 3 2 4 Comparative Example 2 generally 3 4 4 Comparative Example 3 Poor 2 3 3 Comparative Example 4 generally 2 5 2

[0210] From Table 1, it can be seen that the color development ability of the tiles prepared in Examples 6-10 is evaluated as "excellent", indicating that the tiles prepared using the digital glazes of Examples 1-5 are excellent in color expression and can provide richer and more realistic pattern effects.

[0211] The number of pinholes and prickly heat rash on the surfaces of the tiles prepared in Examples 6-10 were all "none", which indicates that the surface of the tiles was very smooth and had no defects.

[0212] The tiles prepared in Examples 6-10 have a wear resistance level of 5, which means that the tiles have extremely high wear resistance, are suitable for use in high-flow or high-wear environments, and can maintain a long service life.

[0213] The ceramic tile prepared in Comparative Example 1 has a "poor" coloring ability, 3 pinholes, 2 prickly heat rashes, and a wear resistance rating of 4. This shows that the ceramic tile prepared without digital glaze is insufficient in color expression, has a certain number of defects on the surface, and has average wear resistance.

[0214] The tile prepared in Comparative Example 2 has "average" coloring ability, 3 pinholes, 4 prickly heat rashes, and a wear resistance rating of 4. Compared with Comparative Example 1, Comparative Example 2 has improved coloring, but has more surface defects and the same wear resistance.

[0215] The ceramic tile prepared in comparative example 3 has "poor" coloring ability, the number of pinholes is 2, the number of prickly heat is 3, and the wear resistance level is 3. The ceramic tile performs poorly in coloring, has fewer surface defects, but has reduced wear resistance.

[0216] The ceramic tile prepared in Comparative Example 4 has "average" coloring ability, 2 pinholes, 5 prickly heat rashes, and a wear resistance rating of 2. The ceramic tile of Comparative Example 4 has average coloring performance, but has the most surface defects and the worst wear resistance.

[0217] The raw materials or reagents used in the examples and comparative examples of the present invention are all purchased from mainstream manufacturers in the market. Those without indicating the manufacturer or concentration are all analytically pure raw materials or reagents that can be routinely obtained. As long as they can play the expected role, there is no special limitation.

[0218] The instruments and equipment used in this embodiment are all purchased from major manufacturers in the market, and there is no particular limitation as long as they can play the expected role. In this embodiment, if no specific technology or conditions are specified, the technology or conditions described in the literature in this field or the product instructions are used. The above embodiments are preferred implementation schemes of the present invention. In addition, the present invention can also be implemented in other ways. Any obvious replacement without departing from the concept of the present invention is within the protection scope of the present invention.

Claims

1. Digital glaze, characterized in that, The invention comprises the following raw materials in parts by weight: 35-45 parts of digital powder, 35-55 parts of solvent, 5-12 parts of dispersant, 5-12 parts of additives; Every 100 parts of the digital powder includes the following raw materials in parts by weight: 35 parts of potassium feldspar, 17 parts of modified quartz, 18 parts of dolomite, 7 parts of corundum, 3 parts of calcined alumina, 7 parts of kaolin, 3 parts of zinc oxide, 10 parts of wear-resistant frit; Every 100 parts of the modified quartz includes the following raw materials in parts by weight: 7 parts of titanium dioxide, 78 parts of quartz sand, 15 parts of color frit; The preparation process of modified quartz is as follows: preparing materials according to the weight composition of 100 parts of modified quartz; adding titanium dioxide and coloring frit into quartz sand, fully mixing, ball milling and sintering, the sintering temperature is 1300-1320°C, and the modified quartz is obtained after the sintering is completed.

2. The digital glaze according to claim 1, characterized in that: The solvent is diisooctyl adipate.

3. The digital glaze according to claim 1, characterized in that: The dispersant includes polyethylene wax and polyvinyl pyrrolidone.

4. The digital glaze according to claim 1, characterized in that: The auxiliary agent is stearic acid polyoxyethylene ether.

5. The digital glaze according to claim 1, characterized in that: The chemical composition of the wear-resistant frit is: CaO: 10.28%, SiO2: 50.06%, Fe2O3: 0.11%, MgO: 3.87%, TiO2: 0.06%, Al2O3: 20.92%, K2O:

0. 23%, Na2O: 2.55%, ZnO: 1%, BaO: 6.71%, SrO: 4.08%, ZrO2: 0.01%, B2O3: 0.03%, Loss: 0.09%.

6. The digital glaze according to claim 1, characterized in that: The chemical composition of the color-producing frit is: CaO: 12.7%, SiO2: 63.47%, Fe2O3: 0.35%, MgO: 1.78%, TiO2: 0.11%, Al2O3: 8.3%, K2O: 4.44%, Na2O: 1.29%, ZnO: 3.4%, BaO: 2.28%, ZrO2: 0.31%, B2O3: 0.97%, PbO: 0.08%, P2O3: 0.29%, Li2O: 0.02%, and Loss: 0.21%.

7. The digital glaze according to claim 3, characterized in that: The weight ratio of polyethylene wax to polyvinyl pyrrolidone in the dispersant is 2:(1-3).

8. The method for preparing the digital glaze according to any one of claims 1 to 7, characterized in that: The following steps are involved: S1. According to the weight composition of the above digital glaze, weigh the corresponding raw materials; S2. The dispersant, additive and part of the solvent are mixed and stirred evenly and then added to the sand mill and continued to stir; S3. Slowly add the digital powder to the sand mill, grind repeatedly until the digital powder is processed to a D90 of 1.0-1.2 μm, then add the remaining solvent, mix thoroughly, and obtain a mixed liquid; S4. The mixed liquid obtained in step S3 is filtered through filter membranes with pore diameters of 10 μm, 5 μm, 3 μm, and 1 μm in sequence, and the filtrate obtained after filtration is the digital glaze.

9. Fine matte ultra-wear-resistant marble tiles, characterized by: The invention comprises the digital glaze described in any one of claims 1 to 7 or the digital glaze prepared by the preparation method described in claim 8.

10. The method for preparing the fine matte super wear-resistant marble tile according to claim 9, characterized in that: The following steps are involved: Preparation of digital glaze; Pour the glaze on the body, print the pattern by inkjet, and then print the digital glaze by inkjet; After high-temperature firing in a kiln, fine matte and ultra-wear-resistant marble tiles are obtained.

Images