Dry granular glaze as well as preparation method and application thereof

Abstract

The invention relates to the technical field of ceramic materials, in particular to dry granular glaze and a preparation method and application thereof.The dry granular glaze is prepared from, by mass, 10-20 parts of dry granules, 5-10 parts of suspension combined material, 0.5-1 part of dispersing agent, 1-2 parts of defoaming agent, 1-2 parts of wetting agent and 70-80 parts of water; the suspension composite material is prepared from the following components in parts by mass: 2 to 5 parts of attapulgite, 2 to 3 parts of sodium carboxymethyl cellulose, 1 to 2 parts of carbomer and 1 to 2 parts of xanthan gum; the mesh number of the dry granules is 80 to 120. According to the dry granular glaze and the preparation method and application thereof, the preparation method is simple, operability is high, and the technical problems that in the prior art, a nozzle works in an overload mode and is blocked are solved on the premise that smoothness and stereoscopic impression of concave-convex textures are considered.

Description

Technical Field

[0001] This invention relates to the field of ceramic materials technology, and in particular to a dry granule glaze, its preparation method, and its application. Background Technology

[0002] To achieve a three-dimensional 3D textured effect on the surface of ceramic tiles, the following manufacturing process is typically used: (1) Using oil-based mold / carving / deep effect ink to spread water-based glaze on the surface of the brick blank to form a textured effect. However, since this process uses the repulsive force between ink and glaze to create a textured effect, this process can achieve a delicate textured effect, but the depth of the texture is limited and the tactile and three-dimensional feel is not strong. (2) After setting a positioning adhesive layer on the glaze surface, dry granules are then spread on the surface of the positioning adhesive layer. After high-temperature sintering, the dry granules form a three-dimensional textured surface. Although this process can achieve a realistic physical texture and a strong tactile feel, it is difficult to achieve a delicate textured surface. In addition, this process has the following defects in practical applications: First, in order to achieve large-area positioning of dry granules, a large amount of adhesive needs to be printed, which can easily lead to overload of the inkjet printer head, resulting in defects such as printhead marks and streaks; Second, dust is easily generated when spreading dry granules, which can easily contaminate the printhead of adjacent inkjet printers and cause printhead blockage.

[0003] Therefore, combining the two types of processes mentioned above, while taking into account the fineness and three-dimensionality of the textured surface, and avoiding the problems of overloading and clogging of the nozzles, has become a development trend in the ceramics industry.

[0004] However, if the two processes are simply combined—first creating a delicate textured surface through the repulsion between oil-based ink and water-based glaze, and then adding dry granules to enhance the three-dimensional effect—the dry granules tend to fill in the depressions of the texture, instead smoothing out the initial texture and failing to achieve the desired enhanced textured effect.

[0005] To address this challenge, the industry has developed a dry granule glaze technology. This dry granule glaze is made by uniformly mixing dry granules with a suspension blend. After glazing, the dry granules naturally form a basic texture within the glaze layer, which is further enhanced by the water-oil repulsion between the dry granules and the subsequently applied oil-based ink. It's important to note that because the dry granules are not applied after the water-oil repulsion between the oil-based ink and water-based glaze has created the texture, the defect of filling in the initial texture during the dry granule application process is avoided. Simultaneously, this process avoids the dependence on inkjet printers found in traditional dry granule positioning processes, effectively solving the technical problems of printhead overload and clogging. However, currently, due to limitations in the selection of dry granule glaze raw material formulations, existing dry granule glazes still have the following drawbacks: (1) The suspension stability of dry particles in dry particle glaze is poor. In order to prevent dry particles from settling, only dry particles with finer particle size (mesh size ≥ 180 mesh) can usually be selected, resulting in limited depth of unevenness after sintering and weak three-dimensionality. (2) The repulsion effect with oil-based ink is weak. Oil-based ink is not easy to effectively separate the dry granules of glaze applied later, resulting in the indistinct fine texture formed by the repulsion of water and oil. The final superimposed texture is still not ideal.

[0006] In summary, existing dry granule glaze technology generally has two limitations: first, it is difficult to make the textured surface both delicate and three-dimensional; second, it is impossible to effectively avoid nozzle overload and clogging during the production process. Summary of the Invention

[0007] The purpose of this invention is to propose a dry granule glaze, its preparation method, and its application. The preparation method is simple and easy to operate, which helps to solve the technical problems of nozzle overload and nozzle clogging in the prior art while taking into account the fineness and three-dimensionality of the texture.

[0008] To achieve this objective, the present invention adopts the following technical solution: A dry granule glaze, calculated by weight, comprises 10-20 parts dry granules, 5-10 parts suspension mixture, 0.5-1 part dispersant, 1-2 parts defoamer, 1-2 parts wetting agent, and 70-80 parts water; The suspended composite material comprises, by weight, 2-5 parts of attapulgite, 2-3 parts of sodium carboxymethyl cellulose, 1-2 parts of carbomer, and 1-2 parts of xanthan gum; The dry granules have a mesh size of 80 to 120.

[0009] Further, calculated by mass percentage, the dry granules include 10-20% of Class I granules with a mesh size ≥80 mesh and <90 mesh, 20-30% of Class II granules with a mesh size ≥90 mesh and <100 mesh, 30-40% of Class III granules with a mesh size ≥100 mesh and <110 mesh, and 10-20% of Class IV granules with a mesh size of 110-120 mesh.

[0010] Furthermore, calculated by mass parts, the dry granule glaze comprises 15 parts dry granules, 8 parts suspension mixture, 0.8 parts dispersant, 1 part defoamer, 1 part wetting agent, and 75 parts water.

[0011] Furthermore, calculated by mass parts, the suspended composite material comprises 3 parts attapulgite, 2 parts sodium carboxymethyl cellulose, 1 part carbomer, and 2 parts xanthan gum.

[0012] Furthermore, the dispersant includes any one of sodium hexametaphosphate, sodium polyacrylate, and polyvinylpyrrolidone.

[0013] Furthermore, the defoamer is a water-based silicone defoamer.

[0014] Furthermore, the wetting agent includes any one of acetylenic diol wetting agents or polyether-modified organosilicon wetting agents.

[0015] A method for preparing dry granule glaze, used to prepare the dry granule glaze as described above, includes the following steps: A. Mix the attapulgite clay of the specified amount with 20% of the specified amount of water evenly, and let it stand for 2-5 hours to obtain the first mixture; B. Add the formula amount of sodium carboxymethyl cellulose, carbomer, and xanthan gum to 30% of the water while continuously stirring. After the addition is complete, a second mixture is obtained. Add the first mixture to the continuously stirred second mixture to obtain the third mixture; The pH of the third mixture was raised to 8-10, stirred until completely transparent, and allowed to stand for 1-2 hours to obtain the fourth mixture; C. Add the prescribed amounts of dispersant, defoamer, wetting agent, and the remaining prescribed amount of water to the fourth mixture to obtain the fifth mixture; D. Add the prescribed amount of dry granules to the fifth mixture, and then ball mill and sieve the mixture to obtain dry granule glaze.

[0016] An application of a dry granule glaze in the preparation of textured ceramic tiles, using the dry granule glaze as described above, and the application method is as follows: Color ink is printed on the surface of the blank layer according to a preset pattern to form an inkjet printing layer; Fine engraving ink is printed on the surface of the inkjet printing layer according to a preset pattern to form a fine engraving ink layer; Dry granule glaze is applied to the surface of the fine ink layer to form a textured layer; After drying, the ceramic tiles are fired in a kiln and then polished to obtain textured ceramic tiles.

[0017] Furthermore, the application amount of the dry granular glaze is 120–135 g / m³. 2 .

[0018] The technical solution provided by this invention may include the following beneficial effects: 1. This technical solution constructs a macroscopic three-dimensional framework through the accumulation of dry particles, and then induces microscopic shrinkage and phase separation by utilizing the water-oil interface repulsion effect, ultimately achieving a combination of three-dimensionality and delicacy in the textured surface, giving the glaze a more natural and layered decorative effect. Furthermore, the dry particles in this technical solution have a mesh size of 80-120 mesh, which is larger than the ≥180 mesh dry particles commonly used in existing technologies, thus enhancing the three-dimensionality of the textured surface.

[0019] 2. The raw materials for the suspension mixture include attapulgite, sodium carboxymethyl cellulose, carbomer, and xanthan gum. The suspension mixture formed from these four raw materials exhibits excellent suspension properties and can stably suspend large-sized dry particles (i.e., coarse dry particles). The specific principle is as follows: After attapulgite is dispersed in water, its nano-sized rod-shaped crystals can overlap and form a rigid three-dimensional framework network that runs through the entire system, providing direct physical support and barrier to the coarse dry particles. Xanthan gum provides extremely high static structural strength and yield value, generating a strong upward supporting force to counteract the gravity of the coarse dry particles. Sodium carboxymethyl cellulose prevents the agglomeration and enlargement of coarse dry particles through steric hindrance. Simultaneously, after neutralization, the elastic three-dimensional network formed by carbomer intertwines and complements the rigid framework of attapulgite and the pseudoplastic structure of xanthan gum, enhancing the strength and toughness of the entire suspension system. The synergistic combination of these four raw materials forms a suspension network that combines physical support, high structural strength, and excellent dispersion stability, enabling long-term suspension of coarse dry particles. Detailed Implementation

[0020] This technical solution provides a dry granule glaze, which, according to the mass fraction, includes 10-20 parts of dry granules, 5-10 parts of suspension mixture, 0.5-1 part of dispersant, 1-2 parts of defoamer, 1-2 parts of wetting agent, and 70-80 parts of water; The suspended composite material comprises, by weight, 2-5 parts of attapulgite, 2-3 parts of sodium carboxymethyl cellulose, 1-2 parts of carbomer, and 1-2 parts of xanthan gum; The dry granules have a mesh size of 80 to 120.

[0021] In order to achieve both the delicacy and three-dimensionality of the textured surface, and to solve the technical problems of nozzle overload and nozzle clogging in the existing technology, this technical solution proposes a dry granule glaze, the raw materials of which include dry granules, suspension mixture, dispersant, defoamer, wetting agent and water.

[0022] Among them, after application and drying, the dry granule glaze itself can form irregular microscopic or macroscopic three-dimensional raised structures on the glaze surface, constituting the skeleton of the texture and providing the most basic three-dimensional effect. Meanwhile, when dry granule glaze is applied to create textures in ceramic tiles, due to the surface energy difference between oil-based sculpting ink and water-based dry granule glaze, in the initial drying stage, the water-based dry granule glaze spreads rapidly on the oil-based sculpting ink. As the solvent evaporates, the water-based dry granule glaze evaporates fastest at the edges (three-phase contact lines), causing the internal solute to migrate and accumulate towards the edges, a typical "coffee ring effect." Simultaneously, due to the low surface energy of the sculpting ink layer, the water-based dry granule glaze does not completely wet it. In the later stages of drying, the water-based dry granule glaze selectively shrinks and aggregates in certain areas, especially at the top and edges of the raised parts. The aforementioned selective shrinkage and aggregation behavior not only enhances the undulations of the original dry granular skeleton, but also induces phase separation and rearrangement of particles within the dry granular glaze at the microscale (down to the micrometer level), thereby generating rich secondary textures.

[0023] Therefore, this technical solution constructs a macroscopic three-dimensional framework through dry particle stacking, and then induces microscopic shrinkage and phase separation by utilizing the water-oil interface repulsion effect, ultimately achieving a combination of three-dimensionality and delicacy in the textured surface, giving the glaze a more natural and layered decorative effect. Simultaneously, the dry particles in this technical solution have a mesh size of 80–120 mesh, which is larger than the ≥180 mesh dry particles commonly used in existing technologies, thus enhancing the three-dimensionality of the textured surface.

[0024] Secondly, the raw materials of the suspension mixture include attapulgite, sodium carboxymethyl cellulose, carbomer, and xanthan gum. The suspension mixture formed from these four raw materials exhibits excellent suspension properties and can stably suspend large-sized dry particles (i.e., coarse dry particles). The specific principle is as follows: After attapulgite is dispersed in water, its nano-sized rod-shaped crystals can overlap and form a rigid three-dimensional framework network that runs through the entire system, providing direct physical support and barrier to the coarse dry particles. Xanthan gum provides extremely high static structural strength and yield value, generating a strong upward supporting force to counteract the gravity of the coarse dry particles. Sodium carboxymethyl cellulose prevents the agglomeration and increase of coarse dry particles through steric hindrance. Simultaneously, after neutralization, the elastic three-dimensional network formed by carbomer intertwines and complements the rigid framework of attapulgite and the pseudoplastic structure of xanthan gum, enhancing the strength and toughness of the entire suspension system. The synergistic combination of these four raw materials forms a suspension network that combines physical support, high structural strength, and excellent dispersion stability, enabling long-term suspension of coarse dry particles.

[0025] Furthermore, while sodium carboxymethyl cellulose, carbomer, and xanthan gum all possess good hydrophilicity, carbomer, due to its high surface tension and certain oleophilicity, can reduce the hydrophilicity of dry granule enamel if used in excessive amounts. By significantly reducing the carbomer addition from the conventional 5-7% to <1.5%, its adverse effects on hydrophilicity are suppressed, thus ensuring good hydrophilicity of the dry granule enamel and laying the foundation for effective water-oil repulsion between it and subsequent oil-based engraving inks.

[0026] Meanwhile, this technical solution also considers the regulation of the rheological behavior of dry granular glaze by the suspension composite material. Excessive content of the high water-retaining component may hinder the physical displacement of the engraving ink onto the dry granular glaze. This technical solution, by limiting the amount of the high water-retaining component carbomer, reduces the excessive elasticity and structural density of the dried granular glaze, preventing it from inhibiting interfacial dynamic reconstruction due to excessive toughness. Based on this, the suspension composite material system uses xanthan gum and attapulgite as the main rheology modifiers, imparting shear-thinning behavior to the glaze slurry, allowing the viscosity of the dry granular glaze to temporarily decrease when subjected to the local shear force of the engraving ink spreading, thus allowing interfacial reconstruction. Furthermore, as mentioned above, this technical solution ensures the hydrophilicity of the dry granular glaze through the use of highly hydrophilic attapulgite, sodium carboxymethyl cellulose, and xanthan gum, guaranteeing a significant tension difference between the water and oil interfaces. The aforementioned thermodynamic driving force causes the engraving ink to spontaneously shrink and dewet during the drying process. Its effect exceeds the physical resistance brought by the glaze structure, thus ensuring that a delicate texture can be formed based on the water-oil repulsion mechanism while achieving stable suspension of dry particles.

[0027] It should be noted that this technical solution requires the combined use of attapulgite, sodium carboxymethyl cellulose, carbomer, and xanthan gum. The reasons are as follows: First, while carbomer can provide suspension by forming a three-dimensional network after neutralization, its high surface tension and certain oleophilicity mean that using only carbomer in the suspension mixture will weaken the hydrophilicity of the dry granules, thus interfering with the water-oil repulsion between the granules and subsequent oil-based inks. Second, although attapulgite and sodium carboxymethyl cellulose provide good hydrophilicity and suspension, the combined system still lacks sufficient static structural strength, limiting its support for the long-term suspension stability of the dry granules. Even with the introduction of a low content of carbomer, it is difficult to completely overcome the structural weakness. Third, the strong hydrophilicity and high molecular chain entanglement ability of xanthan gum can significantly improve the structural viscosity and spatial support strength of the dry granules in a static state, thus ensuring uniform and stable suspension of the dry granules. Simultaneously, the polar properties of xanthan gum also help maintain the hydrophilic state of the entire glaze system, laying the foundation for the subsequent water-oil repulsion process.

[0028] Finally, when the dry granule glaze of this solution is applied to form the textured surface of ceramic tiles, only one application of the dry granule glaze to the surface of the fine ink layer is needed to form a rich textured surface. It can effectively avoid the technical problems of nozzle overload, nozzle clogging and inaccurate alignment that are easy to occur in the existing technology, greatly simplifying the production process, reducing production costs, improving production controllability, and stabilizing production quality.

[0029] To further explain, the dry granules include 10-20% of Class I granules with a mesh size ≥80 and <90, 20-30% of Class II granules with a mesh size ≥90 and <100, 30-40% of Class III granules with a mesh size ≥100 and <110, and 10-20% of Class IV granules with a mesh size of 110-120.

[0030] This technical solution optimizes the gradation of dry particles and mixes dry particles of different sizes to create richer and more natural texture layers, enhancing the three-dimensionality and detail of the texture, and avoiding the weakening of the natural texture of the embossed texture due to the single particle size composition of the dry particles.

[0031] To further explain, the dry granule glaze comprises 15 parts dry granules, 8 parts suspension mixture, 0.8 parts dispersant, 1 part defoamer, 1 part wetting agent, and 75 parts water.

[0032] This technical solution optimizes the addition amount of each raw material in dry granule glaze, so that each raw material in the formula can give full play to its own performance advantages, which is beneficial to improving the texture effect of dry granule glaze.

[0033] To further explain, the suspended composite material, calculated by mass, comprises 3 parts attapulgite, 2 parts sodium carboxymethyl cellulose, 1 part carbomer, and 2 parts xanthan gum.

[0034] This technical solution optimizes the addition amount of each raw material in the suspension mixture, so that each raw material in the formula can give full play to its own performance advantages, which is conducive to improving the suspension effect of the suspension mixture on dry particles.

[0035] To further clarify, the dispersant includes any one of sodium hexametaphosphate, sodium polyacrylate, and polyvinylpyrrolidone.

[0036] Sodium hexametaphosphate, sodium polyacrylate, and polyvinylpyrrolidone can all be used as dispersants to ensure that all raw materials in the formulation are stably dispersed in the dry granule glaze, preventing the raw materials from agglomerating during storage and maintaining the long-term stability of product performance.

[0037] To further clarify, the defoamer is a water-based silicone defoamer.

[0038] Water-based silicone defoamers are highly compatible with water-based systems, effectively defoaming without causing oil spots or pinholes. Therefore, this technical solution preferably uses a water-based silicone defoamer, which helps ensure the performance of the dry granule glaze while achieving defoaming. It should be noted that the water-based silicone defoamer is BYK-024.

[0039] To further clarify, the wetting agent includes any one of acetylenic diol wetting agents or polyether-modified organosilicon wetting agents.

[0040] This technical solution, by optimizing the type of wetting agent, not only reduces the surface tension of dry granular glaze, allowing it to spread and penetrate better into the surface of the engraving ink layer and improve adhesion, but also facilitates the selection of suitable raw materials according to actual needs, thus improving the flexibility of the solution.

[0041] It should be noted that acetylenol wetting agents can be Surfynol 104E and Dynol 604, etc., and the specific types are not limited here; polyether-modified organosilicon wetting agents can be Tego Wet 270, and the specific types are not limited here.

[0042] A method for preparing dry granule glaze, used to prepare the dry granule glaze as described above, includes the following steps: A. Mix the attapulgite clay of the specified amount with 20% of the specified amount of water evenly, and let it stand for 2-5 hours to obtain the first mixture; B. Add the formula amount of sodium carboxymethyl cellulose, carbomer, and xanthan gum to 30% of the water while continuously stirring. After the addition is complete, a second mixture is obtained. Add the first mixture to the continuously stirred second mixture to obtain the third mixture; The pH of the third mixture was raised to 8-10, stirred until completely transparent, and allowed to stand for 1-2 hours to obtain the fourth mixture; C. Add the prescribed amounts of dispersant, defoamer, wetting agent, and the remaining prescribed amount of water to the fourth mixture to obtain the fifth mixture; D. Add the prescribed amount of dry granules to the fifth mixture, and then ball mill and sieve the mixture to obtain dry granule glaze.

[0043] This technical solution optimizes the preparation method of dry granule glaze, following the principle of step-by-step preparation and gradual mixing. This not only effectively avoids excessively high local concentrations and ensures the uniformity and stability of the dry granule glaze, but also promotes stable suspension and uniform dispersion of the dry granules, thereby improving the workability of the dry granule glaze.

[0044] It should be noted that the pH value of the third mixture is raised to 8-10 in this technical solution in order to utilize the alkaline environment to neutralize the acidity of carbomer, allowing the carbomer to fully swell and thicken, thereby achieving a suspension effect.

[0045] An application of a dry granule glaze in the preparation of textured ceramic tiles, using the dry granule glaze as described above, and the application method is as follows: Color ink is printed on the surface of the blank layer according to a preset pattern to form an inkjet printing layer; Fine engraving ink is printed on the surface of the inkjet printing layer according to a preset pattern to form a fine engraving ink layer; Dry granule glaze is applied to the surface of the fine ink layer to form a textured layer; After drying, the ceramic tiles are fired in a kiln and then polished to obtain textured ceramic tiles.

[0046] This technical solution also proposes the application of dry granule glaze in the preparation of textured ceramic tiles, which helps to solve the technical problems of nozzle overload and nozzle clogging in the existing technology while taking into account the fineness and three-dimensionality of the texture.

[0047] To further clarify, the application rate of the dry granule glaze is 120–135 g / m³. 2 .

[0048] This solution also optimizes the amount of dry granule glaze applied, allowing the amount of dry granule glaze to be applied according to actual needs, thus improving the flexibility of the solution.

[0049] The technical solution of the present invention will be further illustrated below through specific embodiments.

[0050] Example 1 In this embodiment, the composition by weight includes 15 parts dry granules, 8 parts suspension mixture, 0.8 parts sodium hexametaphosphate, 1 part water-based silicone defoamer BYK-024, 1 part acetylenol wetting agent Surfynol 104E, and 75 parts water. The suspension mixture by weight includes 3 parts attapulgite, 2 parts sodium carboxymethyl cellulose, 1 part carbomer, and 2 parts xanthan gum. The dry granules by weight percentage include 15% of Class I granules with a mesh size ≥80 mesh and <90 mesh, 30% of Class II granules with a mesh size ≥90 mesh and <100 mesh, 35% of Class III granules with a mesh size ≥100 mesh and <110 mesh, and 20% of Class IV granules with a mesh size of 110-120 mesh. The preparation method of dry granule glaze includes the following steps: A. Mix the attapulgite clay of the formula amount with 20% of the water of the formula amount evenly, and let it stand for 3 hours to obtain the first mixture; B. Add the formula amount of sodium carboxymethyl cellulose, carbomer, and xanthan gum to 30% of the water while continuously stirring. After the addition is complete, a second mixture is obtained. B. Add the first mixture to the continuously stirred second mixture to obtain the third mixture; The pH of the third mixture was raised to 8, stirred until completely transparent, and allowed to stand for 2 hours to obtain the fourth mixture; C. Add the formulated amounts of sodium hexametaphosphate, water-based silicone defoamer BYK-024, acetylenol wetting agent Surfynol 104E, and the remaining formulated amounts of water to the fourth mixture in sequence to obtain the fifth mixture; D. Add the prescribed amount of dry granules to the fifth mixture, and then ball mill and sieve the mixture to obtain dry granule glaze.

[0051] In this embodiment, colored ink is printed on the surface of the body layer according to a preset pattern to form an inkjet printing layer; fine carving ink is printed on the surface of the inkjet printing layer according to a preset pattern to form a fine carving ink layer; dry granule glaze obtained in Example 1 is applied to the surface of the fine carving ink layer to form a textured layer, which is then dried, fired in a kiln, and polished to obtain a textured ceramic tile. The textured surface of the tile has both fineness and three-dimensionality, with rich effects and a strong three-dimensional effect.

[0052] Example 2 In this embodiment, the composition by weight includes 10 parts dry granules, 10 parts suspension mixture, 0.5 parts sodium polyacrylate, 1 part water-based silicone defoamer BYK-024, 1 part acetylenol wetting agent Surfynol 104E, and 80 parts water; the suspension mixture by weight includes 5 parts attapulgite, 2 parts sodium carboxymethyl cellulose, 1 part carbomer, and 1 part xanthan gum; the dry granules by weight percentage include 10% of Class I granules with a mesh size ≥80 mesh and <90 mesh, 30% of Class II granules with a mesh size ≥90 mesh and <100 mesh, 40% of Class III granules with a mesh size ≥100 mesh and <110 mesh, and 20% of Class IV granules with a mesh size of 110-120 mesh. The preparation method of dry granule glaze includes the following steps: A. Mix the attapulgite clay of the formula amount with 20% of the water of the formula amount evenly, and let it stand for 3 hours to obtain the first mixture; B. Add the formula amount of sodium carboxymethyl cellulose, carbomer, and xanthan gum to 30% of the water while continuously stirring. After the addition is complete, a second mixture is obtained. B. Add the first mixture to the continuously stirred second mixture to obtain the third mixture; The pH of the third mixture was raised to 8, stirred until completely transparent, and allowed to stand for 1 hour to obtain the fourth mixture; C. Add the formulated amounts of sodium polyacrylate, water-based silicone defoamer BYK-024, acetylenol wetting agent Surfynol 104E, and the remaining formulated amount of water to the fourth mixture in sequence to obtain the fifth mixture; D. Add the prescribed amount of dry granules to the fifth mixture, and then ball mill and sieve the mixture to obtain dry granule glaze.

[0053] In this embodiment, colored ink is printed on the surface of the body layer according to a preset pattern to form an inkjet printing layer; fine carving ink is printed on the surface of the inkjet printing layer according to a preset pattern to form a fine carving ink layer; dry granule glaze obtained in Example 2 is applied to the surface of the fine carving ink layer to form a textured layer, which is then dried, fired in a kiln, and polished to obtain a textured ceramic tile. The textured surface of the tile has both fineness and three-dimensionality, with rich effects and a strong three-dimensional effect.

[0054] Example 3 In this embodiment, the composition by weight is as follows: 20 parts dry granules, 5 parts suspension mixture, 1 part sodium polyacrylate, 2 parts water-based silicone defoamer BYK-024, 2 parts acetylenol wetting agent Surfynol 104E, and 70 parts water. The suspension mixture by weight is as follows: 2 parts attapulgite, 3 parts sodium carboxymethyl cellulose, 2 parts carbomer, and 2 parts xanthan gum. The dry granules by weight percentage are as follows: 20% of Class I granules with a mesh size ≥80 mesh and <90 mesh, 25% of Class II granules with a mesh size ≥90 mesh and <100 mesh, 40% of Class III granules with a mesh size ≥100 mesh and <110 mesh, and 15% of Class IV granules with a mesh size of 110-120 mesh. The preparation method of dry granule glaze includes the following steps: A. Mix the attapulgite clay of the formula amount with 20% of the water of the formula amount evenly, and let it stand for 4 hours to obtain the first mixture; B. Add the formula amount of sodium carboxymethyl cellulose, carbomer, and xanthan gum to 30% of the water while continuously stirring. After the addition is complete, a second mixture is obtained. B. Add the first mixture to the continuously stirred second mixture to obtain the third mixture; The pH of the third mixture was raised to 9, stirred until completely transparent, and allowed to stand for 2 hours to obtain the fourth mixture; C. Add the formulated amounts of sodium polyacrylate, water-based silicone defoamer BYK-024, acetylenol wetting agent Surfynol 104E, and the remaining formulated amount of water to the fourth mixture in sequence to obtain the fifth mixture; D. Add the prescribed amount of dry granules to the fifth mixture, and then ball mill and sieve the mixture to obtain dry granule glaze.

[0055] Color ink is printed on the surface of the body layer according to a preset pattern to form an inkjet printing layer; fine carving ink is printed on the surface of the inkjet printing layer according to a preset pattern to form a fine carving ink layer; dry granule glaze obtained in Example 3 is applied to the surface of the fine carving ink layer to form a textured layer, which is then dried and fired in a kiln, and polished to obtain a textured tile. The textured surface of the tile has both delicacy and three-dimensionality, with rich effects and a strong three-dimensional effect.

[0056] Comparative Example 1 The preparation method and raw materials of Comparative Example 1 are the same as those of Example 1, except that the suspension composition of Comparative Example 1 contains only carbomer.

[0057] Color ink is printed onto the surface of the body layer according to a preset pattern to form an inkjet printing layer; fine carving ink is then printed onto the surface of the inkjet printing layer according to the preset pattern to form a fine carving ink layer; dry granule glaze obtained in Comparative Example 1 is applied to the surface of the fine carving ink layer to form a textured layer, which is then dried, fired in a kiln, and polished to obtain a textured tile. The textured surface of the tile only has a three-dimensional feel and lacks a delicate feel.

[0058] Comparative Example 2 Comparative Example 2 uses the same preparation method and raw materials as Example 1. The difference is that the suspension composition of Comparative Example 2 uses the suspension composition of the prior art, that is, according to the mass parts, the suspension composition includes 12 parts of sodium carboxymethyl cellulose, 6 parts of methyl ethylene glycol and 4 parts of sodium metaphosphate.

[0059] Color ink is printed onto the surface of the body layer according to a preset pattern to form an inkjet printing layer; fine carving ink is then printed onto the surface of the inkjet printing layer according to the preset pattern to form a fine carving ink layer; dry granule glaze obtained in Comparative Example 2 is applied to the surface of the fine carving ink layer to form a textured layer. After drying, the tile is fired in a kiln and polished to obtain a textured tile. The dry granule glaze has a weak repulsion effect with oil-based ink, and the dry granule glaze is not easy to effectively repel the subsequently applied oil-based ink, resulting in an indistinct fine textured surface formed by water-oil repulsion. The textured surface of the tile has a three-dimensional feel, but the fineness is slightly lacking.

[0060] The technical principles of the present invention have been described above with reference to specific embodiments. These descriptions are merely for explaining the principles of the invention and should not be construed as limiting the scope of protection of the invention in any way. Based on this explanation, those skilled in the art can readily conceive of other specific embodiments of the invention without inventive effort, and these embodiments will all fall within the scope of protection of the present invention.

Claims

1. A dry-granule glaze, characterized in that, The composition, calculated by weight, includes 10-20 parts dry granules, 5-10 parts suspension mixture, 0.5-1 part dispersant, 1-2 parts defoamer, 1-2 parts wetting agent, and 70-80 parts water. The suspended composite material comprises, by weight, 2-5 parts of attapulgite, 2-3 parts of sodium carboxymethyl cellulose, 1-2 parts of carbomer, and 1-2 parts of xanthan gum; The dry granules have a mesh size of 80 to 120.

2. The dry-granule glaze according to claim 1, characterized in that, According to the mass percentage, the dry granules include 10-20% of Class I granules with a mesh size ≥80 mesh and <90 mesh, 20-30% of Class II granules with a mesh size ≥90 mesh and <100 mesh, 30-40% of Class III granules with a mesh size ≥100 mesh and <110 mesh, and 10-20% of Class IV granules with a mesh size of 110-120 mesh.

3. The dry-granule glaze according to claim 1, characterized in that, Based on the mass fractions, the dry granule glaze comprises 15 parts dry granules, 8 parts suspension mixture, 0.8 parts dispersant, 1 part defoamer, 1 part wetting agent, and 75 parts water.

4. The dry-granule glaze according to claim 1, characterized in that, The suspended composite material comprises 3 parts attapulgite, 2 parts sodium carboxymethyl cellulose, 1 part carbomer, and 2 parts xanthan gum, calculated by mass fraction.

5. A dry-granule glaze according to claim 1, characterized in that, The dispersant includes any one of sodium hexametaphosphate, sodium polyacrylate, and polyvinylpyrrolidone.

6. The dry-granule glaze according to claim 1, characterized in that, The defoamer is a water-based silicone defoamer.

7. The dry-granule glaze according to claim 1, characterized in that, The wetting agent includes any one of acetylenic diol wetting agents or polyether-modified organosilicon wetting agents.

8. A method for preparing a dry granular glaze, characterized in that, The preparation of the dry granule glaze as described in any one of claims 1 to 7 includes the following steps: A. Mix the attapulgite clay of the formula amount with 20% of the water of the formula amount evenly, and let it stand for 2-5 hours to obtain the first mixture; B. Add the formula amount of sodium carboxymethyl cellulose, carbomer, and xanthan gum to 30% of the water while continuously stirring. After the addition is complete, a second mixture is obtained. Add the first mixture to the continuously stirred second mixture to obtain the third mixture; The pH of the third mixture was raised to 8-10, stirred until completely transparent, and allowed to stand for 1-2 hours to obtain the fourth mixture; C. Add the prescribed amounts of dispersant, defoamer, wetting agent, and the remaining prescribed amount of water to the fourth mixture to obtain the fifth mixture; D. Add the prescribed amount of dry granules to the fifth mixture, and then ball mill and sieve the mixture to obtain dry granule glaze.

9. The application of a dry-granule glaze in the preparation of textured ceramic tiles, characterized in that, The application method using the dry granule glaze as described in claims 1 to 7 is as follows: Color ink is printed on the surface of the blank layer according to a preset pattern to form an inkjet printing layer; Fine engraving ink is printed on the surface of the inkjet printing layer according to a preset pattern to form a fine engraving ink layer; Dry granule glaze is applied to the surface of the fine ink layer to form a textured layer; After drying, the ceramic tiles are fired in a kiln and then polished to obtain textured ceramic tiles.

10. The application of a dry granule glaze according to claim 9 in the preparation of textured ceramic tiles, characterized in that, The application rate of the dry granule glaze is 120–135 g / m³. 2 .