Digital glaze and preparation method thereof, delicate matte super wear-resistant marble ceramic tile and preparation method thereof

Abstract

The present application relates to the technical field of ceramic tile glazes, 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 present application discloses a digital glaze, which comprises the following raw materials in parts by weight: 35-45 parts of digital powder, 35-55 parts of solvent, 5-12 parts of dispersing agent, and 5-12 parts of additive; every 100 parts of the 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 clinker; the digital glaze has the advantages of good color development, fine hand feeling, no pinholes and good wear resistance, and greatly improves the quality of marble ceramic tile products.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of ceramic tile glazes, in particular to a digital glaze and a preparation method thereof, and a fine matte super wear-resistant marble ceramic tile and a preparation method thereof. BACKGROUND

[0002] In the building ceramic industry, the glazes used in the traditional bell-shaped glaze spraying and spray gun glazing processes are pure water glazes, which can seriously affect the body strength of large-size super-thin marble ceramic tile products after glazing, leading to easy cracking during the firing process or easy breaking during the later processing.

[0003] As a solid-liquid mixture, the digital glaze replaces pigments, printing oil, printing glaze and other additives, and has the advantages of increasing the richness of patterns and improving the clarity, and can be adjusted according to different kiln temperatures, different hand feelings, gloss, and transparency. The processing process, solvent material, and application performance are very close to ink, and the digital glaze can be printed on the surface of the ceramic tile through the inkjet head, which not only saves the amount of glaze, but also makes the glaze thickness uniform. In addition, the digital glaze is an oily or low-oily substance with low water content, which reduces the impact on the strength of the tile body, and does not produce defects such as glaze marks during sintering.

[0004] However, the current ceramic digital glaze still has defects such as color difference, not enough fine matte, pinhole and acne on the glaze surface, and poor wear resistance.

[0005] Therefore, the present application provides a digital glaze and a preparation method thereof, and a fine matte super wear-resistant marble ceramic tile and a preparation method thereof. SUMMARY

[0006] The present application provides a digital glaze and a preparation method thereof, and a fine matte super wear-resistant marble ceramic tile and a preparation method thereof, which has the advantages of good color development, fine hand feeling, no pinhole and acne, and good wear resistance, greatly improving the quality of marble ceramic tile products.

[0007] The technical scheme adopted by the present application to solve the technical problems is:

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

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

[0010] The digital glaze comprises the following raw materials by weight per 100 parts of digital powder:

[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, and 10 parts of wear-resistant clinker;

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

[0013] Titanium white 7 parts, quartz sand 78 parts, colorant frit 15 parts;

[0014] The preparation process of the modified quartz is as follows: raw materials are prepared according to the weight parts of 100 parts of modified quartz; titanium white and colorant frit are added to the quartz sand, and after being fully mixed, ball milling and sintering are performed, the sintering temperature is 1300-1320℃, and the modified quartz is obtained after sintering is completed.

[0015] In some embodiments, the solvent is diisooctyl adipate.

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

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

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

[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 colorant frit is as follows:

[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 and polyvinylpyrrolidone in the dispersant is 2:(1-3).

[0023] In a second aspect, the application provides a preparation method of the digital glaze, including the following steps:

[0024] Raw materials are prepared according to the weight parts of the digital powder;

[0025] Wet ball milling each single raw material of the digital powder to process to D99<5um, drying;

[0026] According to the weight part, the corresponding digital powder is prepared by mixing;

[0027] The dispersant, the auxiliary agent and part of the solvent are mixed and stirred uniformly, the digital powder is added for ball milling, the ball milling is performed to D90 reaching 1.0-1.2um, then the remaining solvent is added;

[0028] Filtering is performed to obtain the digital glaze.

[0029] In a third aspect, the application provides a fine matte super wear-resistant marble ceramic tile, characterized in that it comprises the digital glaze described above.

[0030] In a fourth aspect, the application provides a preparation method of the fine matte super wear-resistant marble ceramic tile, comprising the following steps:

[0031] Preparation of the digital glaze;

[0032] Spraying the top glaze on the body, performing inkjet printing of the pattern, and then performing inkjet printing of the digital glaze;

[0033] High-temperature firing in a kiln to obtain the fine matte super wear-resistant marble ceramic tile.

[0034] The application has the following beneficial effects:

[0035] 1. The digital glaze described in the application solves the problem that the traditional glazing process (such as bell jar glazing and spray gun glazing) cannot be used for large-size super-thin marble ceramic tile products, and develops a digital glaze and a preparation method thereof that can use a full-digital spray glazing process, breaking the monopoly of foreign technology.

[0036] 2. The existing commercially available digital glaze is prone to color difference, rough and not fine glaze surface, pinhole and other defects on the glaze surface, and poor wear resistance. In view of the above problems, the digital glaze described in the application improves 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 clinker to improve the color development of the digital glaze and increase its use temperature range, thereby preparing a digital glaze with good color development, fine hand feeling, no pinholes and high wear resistance, greatly improving the quality and grade of marble ceramic tile products.

[0037] 3. The digital glaze preparation method of the application has better compatibility of the digital glaze through multi-stage filtration, is not prone to ink dripping, ensures that the particles in the finally obtained product through filtration are within the standard range, does not block the filter of the inkjet printer, and has a longer storage time. BRIEF DESCRIPTION OF DRAWINGS

[0038] The application will be further described below in conjunction with the drawings and examples.

[0039] Figure 1 Process flow chart for the method of preparing the digital glaze described in the present application. DETAILED DESCRIPTION

[0040] For the convenience of those skilled in the art, the present application is further described below in conjunction with examples, and the content mentioned in the embodiments is not a limitation of the present application.

[0041] As used herein, "and / or", includes the term "and", the term "or" and any combinations thereof. The terms used herein are used only to describe particular embodiments, and are not intended to limit the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms, unless the context clearly indicates otherwise. It will be further understood that the term "comprises" when used in this specification, specifies the presence of stated features, integers, steps, operations, elements, and / or components, but does not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups 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 this application belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.

[0043] The exemplary applications described herein can suitably lack any one or more of the elements described herein, and such applications should not be deemed outside the scope of the present application, even if one or more of the elements of the applications described herein are not present. Thus, the terms "comprise", "comprises", "comprising", "including", "includes" or any other variation thereof are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises, includes or consists of any combination of elements as recited in the claims are within the scope of the present application. Additionally, the terms "comprise", "comprises", "comprising", "including", "includes" or any other variation thereof are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises, includes or consists of any combination of elements as recited in the claims are within the scope of the present application. Additionally, the use of the term "about" in the context of the present application is intended to cover any variation that is within the scope of the intended application. Thus, the term "about" is intended to cover variations that are within the experimental error of the measurements or the skill in the art, or variations that occur due to reasonable expectation variations. The term "consisting essentially of will be construed as consisting of the specified features or steps plus any non-essential feature or step.

[0044] Terminology:

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

[0046] Body refers to the semi-finished product obtained after the pressing forming process in the production process of ceramic products. The body is usually made of ceramic raw materials (such as clay, quartz, feldspar, etc.) through mixing, forming (such as pressing, slip casting, etc.) and other processes. In the production of ceramic tiles, the body is the basis of the final product, various glazes will be applied on it and sintered to obtain finished ceramic tiles with decorative and functional properties.

[0047] Face glaze is a layer of glaze applied on the surface of ceramic body, mainly for decoration and protection. Face glaze can give ceramic products rich color, luster and texture, while resisting wear, corrosion and other external factors, prolonging the service life of ceramic products. In this application, the preparation method of fine matte super wear-resistant marble ceramic tile first applies face glaze on the body, then prints patterns and digital glaze by inkjet printing to form the final decorative effect.

[0048] Inkjet printing pattern is a technology that uses inkjet printers to directly print patterns on ceramic body or glaze surface. In the production of ceramic tiles, inkjet printing technology can achieve highly personalized pattern design and color expression, improving the added value of products. The process of inkjet printing pattern usually involves accurately spraying ink containing pigments through the nozzle onto the body or glaze surface to form fine patterns and color levels. In this application, the preparation method of fine matte super wear-resistant marble ceramic tile, inkjet printing pattern is the next process after applying face glaze, which is used to further beautify the appearance of ceramic tile.

[0049] In view of the problems of existing commercial digital glaze, such as color difference, rough and not delicate glaze surface, pinhole and acne defects, and poor wear resistance, the application provides a digital glaze, which comprises the following raw materials by weight:

[0050] Digital powder 35-45 parts, solvent 35-55 parts, dispersant 5-12 parts, additive 5-12 parts;

[0051] The digital powder comprises the following raw materials by weight per 100 parts:

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

[0053] The modified quartz comprises the following raw materials by weight per 100 parts of modified quartz:

[0054] Titanium dioxide 7 parts, quartz sand 78 parts, color-developing clinker 15 parts;

[0055] The preparation process of the modified quartz is as follows: raw materials are prepared according to the weight parts of 100 parts of modified quartz; titanium dioxide and color-developing clinker are added to the quartz sand, and after being fully mixed, ball milling and sintering are performed, the sintering temperature is 1300-1320℃, and the modified quartz is obtained after the sintering is completed.

[0056] It can be understood that the digital powder is the main material of the digital glaze, which contains potassium feldspar, modified quartz, dolomite, corundum and other minerals and compounds. These raw materials are processed through specific proportioning to form a powder with specific chemical composition and physical properties, which provides the digital glaze with the required basic properties such as color, gloss, wear resistance, etc.; specifically, potassium feldspar and dolomite can be used as fluxing agents to reduce the melting temperature of the glaze; corundum and calcined alumina can improve the hardness and wear resistance of the glaze layer; and the modified quartz can improve the color-developing ability and gloss of the glaze through its special chemical composition and physical properties.

[0057] In the present application, the weight parts of the digital powder are 35-45 parts (including the end point value), for example, it can be 35 parts, 37 parts, 40 parts, 41 parts, and the appropriate weight parts of the 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 and have poor fluidity, making it difficult to apply evenly; at the same time, too much powder will also increase the thickness of the glaze layer and the sintering difficulty, which is easy to cause the glaze to crack or blister. On the contrary, if the digital powder is too little, the glaze layer will be too thin, it is difficult to form a stable glaze surface, and the color, gloss and wear resistance will be affected.

[0058] Specifically, the titanium dioxide and color-developing agent in the modified quartz undergo a chemical reaction with the 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 surface. At the same time, the color-developing clinker in the modified quartz can also promote the uniform distribution and brightness of the glaze color, making the ceramic tile have better decorative effect. The prepared modified quartz can improve the wear resistance, chemical corrosion resistance and color-developing 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, the corresponding weight parts of quartz sand, titanium white and colorant ingot are weighed; the titanium white and colorant ingot are added to the quartz sand, and then the mixture is fully mixed and ball milled for 2-3 hours; the ball milled mixture is sintered at a temperature of 1300-1320 DEG C for 0.8-1.2 hours to obtain the modified quartz.

[0060] In some embodiments, the solvent is diisooctyl adipate. The solvent mainly serves to improve the stability of the ink, so that the viscosity, surface tension and the like of the ink are not easily changed with temperature. The selection of the solvent has an important influence on the flowability, drying speed, sintering performance and the like of the glaze. Diisooctyl adipate has good dissolving capacity and volatility, and can effectively disperse the digital powder uniformly in 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, and further affects the final quality of the ceramic tile.

[0061] In the present application, the weight parts of the solvent are 35-55 (including the end point value), for example, can be 35 parts, 37 parts, 40 parts, 45 parts, 48 parts, 55 parts, and an 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 layer thickness, affecting the color, gloss and wear resistance of the ceramic tile; at the same time, too much solvent will also increase the drying time and energy consumption in the sintering process. If the solvent is too little, the glaze is too thick, it is difficult to apply the glaze uniformly, and defects such as pinholes and bubbles are easily generated.

[0062] In some embodiments, the dispersant includes polyethylene wax and polyvinylpyrrolidone. The dispersant mainly serves to prevent the digital powder from agglomerating and precipitating in the solvent, and to maintain the uniformity and stability of the glaze. The dispersant such as polyethylene wax and polyvinylpyrrolidone adsorbs on the surface of the digital powder particles through its unique molecular structure and surface properties, forming a protective film to prevent direct contact and agglomeration between the particles. In the present application, the weight parts of the dispersant are 5-12 (including the end point value), for example, can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 12 parts, and an appropriate amount of dispersant can maintain the uniformity and stability of the glaze, while preventing agglomeration and precipitation between the particles. Too much dispersant may cause the glaze to be too viscous, affecting the flowability; 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, it cannot effectively prevent the agglomeration and precipitation of the digital powder, resulting in uneven and unstable glaze.

[0063] Specifically, the weight ratio of polyethylene wax to polyvinylpyrrolidone in the dispersant is 2:(1-3). The appropriate ratio of polyethylene wax to polyvinylpyrrolidone helps to improve the dispersing effect.

[0064] In some embodiments, the auxiliary agent is polyoxyethylene stearate. The auxiliary agent has good emulsifying and thickening properties, and can increase the interaction between the powder particles and the solvent, making the glaze system more stable.

[0065] In the present application, the amount of auxiliary agent is 5-12 parts (including end values), for example, it can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 12 parts. An appropriate amount of auxiliary agent can increase the interaction between the powder particles and the solvent, making the glaze system more stable. Too much auxiliary agent can make the glaze too thick, affecting the flowability; if the auxiliary agent is too little, it cannot effectively prevent the agglomeration 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 aluminum oxide (Al2O3) and various wear-resistant components, which can form a high-hardness glaze layer during sintering, thereby significantly improving the wear resistance of the ceramic tile surface; through the specific chemical composition of the wear-resistant frit, it has good thermal stability, chemical corrosion resistance, high wear resistance and high hardness, and can also improve the color development effect of the inkjet pattern.

[0068] In some embodiments, the chemical composition of the color-developing 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-developing frit has strong gloss, high transparency, and strong fluxing effect, and can form a glass phase during sintering, thereby improving the transparency and gloss of the glaze surface, and promoting the uniform distribution and brightness of the glaze color.

[0071] The preparation method of 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 < 5 μm, and then sieved (sieved through a 325 mesh screen) and dried (each of the powders has a water content of less than 0.1%)

[0073] The corresponding digital powder is prepared by mixing according to weight parts;

[0074] The dispersant, the auxiliary agent and part of the solvent are mixed and stirred uniformly, and the digital powder is added for ball milling, and the ball milling is performed until D90 reaches 1.0-1.2 μm, and then the remaining solvent is added;

[0075] Filtration is performed to obtain the digital glaze.

[0076] The specific process is as follows: S1, each single raw material in the digital powder is wet ball milled to process each raw material to D99 < 5 μm, and then sieved;

[0077] S2, each powder sieved in the step S1 is dried;

[0078] S3, each powder dried in the step S2 is added into a high mixer according to the proportion of the digital powder for mixing to obtain the digital powder;

[0079] S4, the dispersant, the auxiliary agent and part of the solvent are mixed and stirred uniformly, and then added into a sand mill for continuous stirring;

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

[0081] S6, the mixture obtained in the step S5 is filtered through a filter hole, and the digital glaze is obtained after filtration.

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

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

[0084] In the step S3, the mixing time of each of the powders in the high mixer is 20-30 min, and the rotation speed is 100-150 revolutions per minute;

[0085] In the step S5, the sand milling time of each of the powders in the sand mill is 2-10 h, and after sand milling, D90 of each of the powders reaches 1.0-1.2 um.

[0086] In step S5, the digital glaze ink is filtered through filter membranes with filter hole diameters of 10 μm, 5 μm, 3 μm and 1 μm in sequence, and the final filtrate is the digital glaze ink for full-digital glaze spraying.

[0087] The preparation method of the fine matte super wear-resistant marble ceramic tile comprises the following steps:

[0088] Preparation of digital glaze;

[0089] Spraying of top glaze on the body, inkjet printing of patterns, and inkjet printing of digital glaze;

[0090] High-temperature firing in a kiln to obtain the fine matte super wear-resistant marble ceramic tile.

[0091] Specifically, the preparation process of the 1600 mm*3200 mm specification digital glaze ceramic tile is as follows: pressing a body using a conventional ceramic body material → spraying a conventional top glaze on the body → inkjet printing of patterns → inkjet printing of digital glaze → high-temperature firing in a kiln to obtain a marble ceramic tile.

[0092] More specifically, the conventional top glaze is sprayed on the body, and a suitable top glaze formula (a common top glaze) is selected, and the viscosity, fluidity and drying speed of the top glaze need to be matched with the characteristics of the body; the top glaze is uniformly sprayed on the surface of the body using an automatic glaze spraying device to ensure that the entire surface is covered with the top glaze and has a uniform thickness. After glazing, the body needs to be pre-dried to remove the water in the top glaze and form a uniform glaze surface;

[0093] Inkjet printing of patterns, the process being as follows: according to design requirements, a professional inkjet printing device is used to directly print patterns on the dried top glaze, and after printing, appropriate solidification or drying treatment is performed;

[0094] Inkjet printing of digital glaze, the process being as follows: according to different change requirements of the glossiness and hand feeling of the ceramic tile surface, single-channel or double-channel inkjet printing is selected, and the channel gray scale is generally between 30-90% for inkjet printing of digital glaze;

[0095] High-temperature firing in a kiln, the process being as follows: the ceramic tile on which the digital glaze is printed is sent into a kiln for high-temperature firing at 1170-1220 ℃, and the firing period is 50-60 minutes.

[0096] Preparation Example 1

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

[0098] 7 parts of titanium white, 78 parts of quartz sand and 15 parts of color-developing frit;

[0099] The preparation process of the modified quartz is as follows: preparing materials according to the weight parts of 100 parts of the modified quartz; adding titanium white and color-developing frit into the quartz sand, and then ball-milling and sintering after fully mixing, the sintering temperature is controlled at 1300-1320 DEG C, the sintering time is controlled at 0.8-1.2 h, and the modified quartz is obtained after sintering;

[0100] The chemical composition of the color-developing frit is as follows:

[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] The digital powder material includes the following raw materials by weight parts per 100 parts of the digital powder material:

[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 the digital powder material includes the following steps:

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

[0107] According to the weight parts of 100 parts of the digital powder material, the dried powder material is weighed: 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 are added into a high-speed mixer for mixing (for example, the mixing time is 30 min, and the rotating speed is 150 r / min), and the digital powder material is obtained.

[0108] Example 1

[0109] The digital glaze includes the following raw materials by weight parts:

[0110] 35 parts of the digital powder material (Preparation Example 2), 35 parts of diisooctyl adipate, 5 parts of polyethylene wax and polyvinylpyrrolidone, and 5 parts of polyoxyethylene stearate;

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

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

[0113] S2. After the dispersing agent, the auxiliary agent and part of the solvent are uniformly mixed and stirred, they are added into a sand mill for continuous stirring;

[0114] S3. The digital powder is slowly added into the sand mill, and repeated grinding is carried out until the D90 of the digital powder reaches 1.0-1.2 μm, then the remaining solvent is added for sufficient mixing to obtain a mixed liquid;

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

[0116] Example 2

[0117] The digital glaze comprises the following raw materials by weight:

[0118] The digital powder (Preparation Example 2) 45 parts, diisooctyl adipate 55 parts, polyethylene wax and polyvinylpyrrolidone 12 parts, and polyoxyethylene stearate 12 parts;

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

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

[0121] S2. After the dispersing agent, the auxiliary agent and part of the solvent are uniformly mixed and stirred, they are added into a sand mill for continuous stirring;

[0122] S3. The digital powder is slowly added into the sand mill, and repeated grinding is carried out until the D90 of the digital powder reaches 1.0-1.2 μm, then the remaining solvent is added for sufficient mixing to obtain a mixed liquid;

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

[0124] Example 3

[0125] The digital glaze comprises the following raw materials by weight:

[0126] The digital powder (Preparation Example 2) 45 parts, diisooctyl adipate 55 parts, polyethylene wax and polyvinylpyrrolidone 12 parts, and polyoxyethylene stearate 12 parts;

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

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

[0129] S2. After the dispersing agent, the auxiliary agent and part of the solvent are uniformly mixed and stirred, they are added into a sand mill for continuous stirring;

[0130] S3. The digital powder is slowly added into the sand mill, and repeated grinding is carried out until the digital powder is processed to D90 of 1.0-1.2 μm, then the remaining solvent is added for sufficient mixing to obtain a mixed liquid;

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

[0132] Example 4

[0133] The digital glaze comprises the following raw materials by weight part:

[0134] The digital powder (Preparation Example 2) 40 parts, diisooctyl adipate 50 parts, polyethylene wax and polyvinylpyrrolidone 10 parts, and polyoxyethylene stearate 10 parts;

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

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

[0137] S2. After the dispersing agent, the auxiliary agent and part of the solvent are uniformly mixed and stirred, they are added into a sand mill for continuous stirring;

[0138] S3. The digital powder is slowly added into the sand mill, and repeated grinding is carried out until the digital powder is processed to D90 of 1.0-1.2 μm, then the remaining solvent is added for sufficient mixing to obtain a mixed liquid;

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

[0140] Example 5

[0141] The digital glaze comprises the following raw materials by weight part:

[0142] The digital powder (Preparation Example 2) 37 parts, diisooctyl adipate 38 parts, polyethylene wax and polyvinylpyrrolidone 9 parts, and polyoxyethylene stearate 9 parts;

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

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

[0145] S2. After the dispersant, auxiliary agent and part of the solvent are mixed and stirred uniformly, they are added into a sand mill for continuous stirring;

[0146] S3. The digital powder is slowly added into the sand mill, and repeated grinding is performed until the digital powder is processed to D90 of 1.0-1.2 μm, then the remaining solvent is added, and sufficient mixing is performed to obtain a mixed liquid;

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

[0148] Example 6

[0149] The preparation method of the fine matte super wear-resistant marble ceramic tile comprises the following steps:

[0150] The conventional ceramic body is pressed into a body, the conventional face glaze is sprayed on the body, the pattern is inkjet printed, the digital glaze (Example 1) is inkjet printed, and the ceramic tile is obtained after high-temperature firing in a kiln.

[0151] The inkjet printing of the digital glaze is performed by selecting double-channel inkjet printing, and the gray scales of the two channels are both 50%.

[0152] The printed digital glaze completed ceramic tile is sent into a kiln for high-temperature firing at 1220°C, and the firing period is 50 minutes.

[0153] Example 7

[0154] The preparation method of the fine matte super wear-resistant marble ceramic tile comprises the following steps:

[0155] The conventional ceramic body is pressed into a body, the conventional face glaze is sprayed on the body, the pattern is inkjet printed, the digital glaze (Example 2) is inkjet printed, and the ceramic tile is obtained after high-temperature firing in a kiln.

[0156] Example 8

[0157] The preparation method of the fine matte super wear-resistant marble ceramic tile comprises the following steps:

[0158] The conventional ceramic body is pressed into a body, the conventional face glaze is sprayed on the body, the pattern is inkjet printed, the digital glaze (Example 3) is inkjet printed, and the ceramic tile is obtained after high-temperature firing in a kiln.

[0159] Example 9

[0160] The preparation method of the fine matte super wear-resistant marble ceramic tile comprises the following steps:

[0161] Using conventional ceramic blank to press into a green body → Spraying conventional surface glaze on the green body → Inkjet printing pattern → Inkjet printing digital glaze (Example 4) → After high-temperature firing in a kiln, ceramic tile is obtained.

[0162] Example 10

[0163] The preparation method of the fine matte super wear-resistant marble ceramic tile comprises the following steps:

[0164] Using conventional ceramic blank to press into a green body → Spraying conventional surface glaze on the green body → Inkjet printing pattern → Inkjet printing digital glaze (Example 5) → After high-temperature firing in a kiln, ceramic tile is obtained.

[0165] Comparative Example 1

[0166] The preparation method of the marble ceramic tile comprises the following steps:

[0167] Using conventional ceramic blank to press into a green body → Spraying conventional surface glaze on the green body → Inkjet printing pattern → After high-temperature firing in a kiln, ceramic tile is obtained.

[0168] After high-temperature firing in a kiln, the process is: the ceramic tile on which the digital glaze is printed is sent into the kiln, and high-temperature firing is carried out at 1220℃, and the firing period is 50 minutes.

[0169] Comparative Example 2

[0170] The digital powder comprises the following raw materials by weight per 100 parts:

[0171] 35 parts of potash 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 clinker;

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

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

[0174] According to the weight parts of 100 parts of the digital powder, the dried powder is weighed: 35 parts of potash 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 clinker are added into a high-speed mixer for mixing (for example, the mixing time is 30 minutes, and the rotating speed is 150 revolutions per minute), and the digital powder is obtained.

[0175] The digital glaze comprises the following raw materials by weight:

[0176] Digital powder 35 parts, diisooctyl adipate 35 parts, polyethylene wax and polyvinyl pyrrolidone 5 parts, polyoxyethylene stearate 5 parts; the specific preparation method is consistent with example 1;

[0177] Marble tile, the specific preparation method is consistent with example 6;

[0178] Comparative example 3

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

[0180] Titanium dioxide 7 parts, quartz sand 93 parts;

[0181] The preparation process of modified quartz is as follows: according to the weight parts of 100 parts of modified quartz, the raw materials are prepared; titanium dioxide is added to the quartz sand, and after being mixed thoroughly, it is ball milled and sintered, the sintering temperature is controlled at 1300-1320℃, the sintering time is controlled at 0.8-1.2h, and the modified quartz is obtained after sintering;

[0182] The digital powder includes the following raw materials by weight per 100 parts:

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

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

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

[0186] According to the weight parts of 100 parts of digital powder, the dried powder is weighed: potassium feldspar 35 parts, modified quartz 17 parts, dolomite 18 parts, corundum 7 parts, calcined alumina 3 parts, kaolin 7 parts, zinc oxide 3 parts, and wear-resistant clinker 10 parts are added to the high-speed mixer for mixing (for example, the mixing time is 30min, and the rotating speed is 150r / min), and the digital powder is obtained.

[0187] The digital glaze includes the following raw materials by weight:

[0188] Digital powder (preparation example 2) 35 parts, diisooctyl adipate 35 parts, polyethylene wax and polyvinyl pyrrolidone 5 parts, polyoxyethylene stearate 5 parts; the specific preparation method of digital glaze is consistent with example 1;

[0189] Marble tile, the specific preparation method is consistent with example 6;

[0190] Comparative example 4

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

[0192] Titanium white 7 parts, quartz sand 78 parts, colorant frit 15 parts;

[0193] The preparation process of modified quartz is as follows: raw materials are prepared according to the weight parts of 100 parts of modified quartz; titanium white, colorant frit are added to the quartz sand, and after being fully mixed, ball milling and sintering are carried out, the sintering temperature is controlled at 1300-1320℃, the sintering time is controlled at 0.8-1.2h, and the modified quartz is obtained after sintering is completed;

[0194] The chemical composition of the colorant frit is as follows:

[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] The digital powder material includes the following raw materials by weight parts per 100 parts:

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

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

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

[0200] According to the weight parts of 100 parts of the digital powder material, the dried powder material is weighed: potassium feldspar 45 parts, modified quartz 17 parts, dolomite 18 parts, corundum 7 parts, calcined alumina 3 parts, kaolin 7 parts, and zinc oxide 3 parts, which are added to a high-speed mixer for mixing (for example, the mixing time is 30 minutes and the rotation speed is 150 revolutions per minute), to obtain the digital powder material.

[0201] The digital glaze includes the following raw materials by weight parts:

[0202] Digital powder material (preparation example 2) 35 parts, diisooctyl adipate 35 parts, polyethylene wax and polyvinylpyrrolidone 5 parts, and polyoxyethylene stearate 5 parts; the specific preparation method of the digital glaze is consistent with example 1;

[0203] Marble tiles, prepared according to the consistent method and 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 were summarized in Table 1 below:

[0205] Color development: color card contrast color development;

[0206] Pinholes and pimples, the number of statistics to represent;

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

[0208] Table 1

[0209] Color development Pinhole number Pimple number 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 Fair 3 4 4 Comparative Example 3 Poor 2 3 3 Comparative Example 4 Fair 2 5 2

[0210] From Table 1, it can be seen that the tiles prepared in Examples 6-10 have a color development evaluation of "excellent", which shows that the tiles prepared using the digital glaze of Examples 1-5 have very good color performance and can provide more rich and realistic pattern effects.

[0211] The number of pinholes and pimples on the surface of the tiles prepared in Examples 6-10 is "none", which shows that the surface of the tiles is very smooth and has no defects.

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

[0213] The tiles prepared in Comparative Example 1 have a color development of "poor", a pinhole number of 3, a pimple number of 2, and a wear resistance of 4. This shows that the tiles prepared without digital glaze have insufficient color performance, a certain number of surface defects, and general wear resistance.

[0214] The tiles prepared in Comparative Example 2 have a color development of "general", a pinhole number of 3, a pimple number of 4, and a wear resistance of 4. Compared with Comparative Example 1, Comparative Example 2 has improved color development, but more surface defects and the same wear resistance.

[0215] The tiles prepared in Comparative Example 3 have a color development of "poor", a pinhole number of 2, a pimple number of 3, and a wear resistance of 3. The tiles have poor color performance, fewer surface defects, but reduced wear resistance.

[0216] The tile prepared by Comparative Example 4 has a "general" color development ability, 2 pinholes, 5 pimples, and a wear resistance grade of 2. The tile of Comparative Example 4 has a general color development, 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 application are purchased from mainstream manufacturers in the market. If the manufacturer is not specified or the concentration is not specified, it is an analytical grade raw material or reagent that can be obtained conventionally, and is not particularly limited as long as it can play the expected role.

[0218] The instruments and equipment used in the examples are purchased from major manufacturers in the market, and are not particularly limited as long as they can play the expected role. If the specific technology or condition is not specified in the examples, it is performed according to the technology or condition described in the literature in the art or according to the product instruction. The above examples are the preferred implementation scheme of the present application, and the present application can also be implemented in other ways without departing from the concept of the present application. Any obvious substitution within the scope of the present application is within the protection scope of the present application.

Claims

1. A digital glaze, characterized in that, Including the following parts by weight of raw materials: The mixture comprises 35-45 parts digital powder, 35-55 parts solvent, 5-12 parts dispersant, and 5-12 parts additives; the solvent is diisooctyl adipate; the dispersant includes polyethylene wax and polyvinylpyrrolidone; and the additive is polyoxyethylene stearate. Each 100 parts of the digital powder comprises the following parts by weight of raw materials: The composition includes 35 parts potassium feldspar, 17 parts modified quartz, 18 parts dolomite, 7 parts corundum, 3 parts calcined alumina, 7 parts kaolin, 3 parts zinc oxide, and 10 parts wear-resistant frit; the chemical composition of the wear-resistant frit is as follows: 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%; Each 100 parts of the modified quartz comprises the following parts by weight of raw material: 7 parts titanium dioxide, 78 parts quartz sand, and 15 parts color-developing frit; the chemical composition of the color-developing frit is as follows: 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%; The preparation process of modified quartz is as follows: prepare materials according to 100 parts by weight of modified quartz; add titanium dioxide and color-developing frit to quartz sand, mix thoroughly, ball mill, and sinter at a temperature of 1300-1320℃. Modified quartz is obtained after sintering.

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

3. The method for preparing digital glaze according to any one of claims 1-2, characterized in that, Includes the following steps: S1. Weigh the corresponding raw materials according to the above-mentioned digital glaze composition by weight; S2. Mix the dispersant, additives and part of the solvent evenly, then add the mixture into the sand mill and continue stirring. S3. Slowly add digital powder to the sand mill and grind repeatedly until the digital powder is processed to D90 of 1.0-1.2μm. Then add the remaining solvent and mix thoroughly to obtain a mixed liquid. S4. The mixture obtained in step S3 is filtered sequentially through filter membranes with pore diameters of 10μm, 5μm, 3μm, and 1μm. The filtrate obtained after filtration is digital glaze.

4. Fine-grained matte, ultra-wear-resistant marble-look ceramic tile, characterized in that... This includes the digital glaze as described in any one of claims 1-2 or the digital glaze prepared by the preparation method described in claim 3.

5. The method for preparing fine matte ultra-wear-resistant marble ceramic tiles according to claim 4, characterized in that, Includes the following steps: Preparation of digital glaze; A top glaze is applied to the blank, and then an inkjet printed pattern is created. Finally, a digital glaze is printed using inkjet printing. After being fired at high temperatures in a kiln, a delicate, matte, and ultra-wear-resistant marble tile is obtained.

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