A soft light skin-feeling glaze, a soft light skin-feeling ceramic rock plate with a digital three-dimensional effect, and a preparation method thereof

Abstract

The present invention relates to the technical field of ceramic rock slab production, and specifically to a soft-light skin-feeling glaze, a soft-light skin-feeling ceramic rock slab with a digital three-dimensional effect, and a preparation method thereof. The formulas of the blank, soft-light base glaze, and soft-light surface glaze in the present invention all belong to clay minerals with good plasticity. At the same time, adding a toughening composition to the blank can greatly enhance the strength and toughness of the ceramic rock slab blank. The toughening composition has a certain adhesiveness and can form a bridge between ceramic particles to enhance the bonding force between particles. During the drying process of the blank, this bonding effect helps to maintain the relative position of the particles, reduce the movement and agglomeration of the particles, thereby forming a more uniform and dense microstructure and improving the toughness of the ceramic rock slab. The present invention also effectively eliminates stress in the firing process through step-by-step temperature increase firing, improves the firing qualification rate, and reduces cracking, and has broad application prospects.

Description

Technical Field

[0001] The present invention relates to the technical field of ceramic rock slab production, and in particular to a soft-light skin-feeling glaze, a soft-light skin-feeling ceramic rock slab with a digital three-dimensional effect, and a preparation method thereof. Background Art

[0002] As a new type of ceramic product, ceramic rock slabs, with their extra-large specifications, can carry richer textural elements than traditional ceramic tiles. Combined with advanced technology, they can achieve high-bending and high-strength green quality. Ceramic rock slabs have the advantages of simple and elegant decorative effects, fewer seams, avoidance of dirt and grime, and high construction and paving efficiency. Ceramic rock slabs have a Mohs hardness of over 6, are scratch-resistant and wear-resistant, and are not easily scratched by sharp objects, making them suitable for easily worn areas such as kitchen countertops. They are fired at temperatures above 1200°C and meet A1 fire protection standards. They do not change color, emit smoke, or release harmful substances when burned with open flames, and can be used in high-temperature environments such as near stoves. The surface porosity is almost zero, the water absorption rate is low, stains are difficult to penetrate, and they are easy to clean. The stain resistance level reaches the Class 5 hygiene standard.

[0003] Soft Glow Skin-Touch Glaze is a glaze applied to ceramic rock slabs, imparting a soft sheen and delicate touch, resembling a skin-like texture. Its glossiness typically ranges from 15-30 degrees, reducing reflectivity and visual pollution, offering visual comfort. Soft Glow Skin-Touch Ceramic Rock Slabs with Digital 3D Effects are based on ceramic rock slabs and combine Soft Glow Skin-Touch Glaze with digital 3D technology. It combines the advantages of Soft Glow Skin-Touch Glaze with the precise control of texture and pattern through digital technology, creating a unique 3D effect that adds depth and realism to the surface texture.

[0004] Although ceramic rock slabs have high hardness, they are brittle and easily crack or break when subjected to large external impacts, especially thinner rock slabs, which have limited load-bearing capacity. For example, patent document CN110627532A discloses a large-scale ceramic rock slab and its production process. The raw materials used in the rock slab blanks are composed of: 40%-55% medium-temperature sand, 15%-25% low-temperature sand, 16%-25% ball clay, 5%-10% burned talc, 2%-5% calcined kaolin and 1%-3% zirconium silicate. It has realistic simulated 3D texture, delicate texture and hardness. However, the blank formula basically follows the traditional formula, with less clay mineral raw materials, poor plasticity, low blank strength, high brittleness and easy cracking during secondary processing.

[0005] Patent technology document CN115536372B discloses a ceramic rock plate, a dry powdered ceramic rock plate blank and a preparation method thereof, comprising the following components in parts by weight: 0.1-0.5 parts of sodium hexametaphosphate, 0.1-0.5 parts of fumed nano-alumina, 0.2-0.8 parts of precipitated nano-silicon dioxide; and further comprising the following components in parts by weight: 4-8 parts of calcined coal gangue, 4-10 parts of bauxite, 8-16 parts of potassium sodium water abrasive, 2-6 parts of pyrophyllite, 13-23 parts of potassium sand, potassium sodium 10-30 parts of mixed sand, 10-20 parts of silica sand, 5-17 parts of bentonite, and 2-6 parts of diopside are selected and compounded to ensure that the dry pulverization is carried out smoothly and the green body has sufficient strength. However, the powder particles obtained by dry pulverization have a rough and irregular surface, a narrow particle size distribution range, and coarse particles, which makes it difficult for the powder to be tightly packed during the pressing process. The internal porosity of the green body is high and the structure is not dense enough, thereby reducing the strength and toughness of the green body and making it prone to cracking.

[0006] Therefore, according to the relevant technologies mentioned above, there is an urgent need to develop a soft-light skin-feeling glaze, a soft-light skin-feeling ceramic rock plate with a digital three-dimensional effect and a preparation method thereof. Summary of the Invention

[0007] In view of this, the purpose of the present invention is to propose a soft-light skin-feel glaze, a soft-light skin-feel ceramic rock plate with a digital three-dimensional effect and a preparation method thereof, so as to solve the problems of low toughness, brittle texture and easy cracking of ceramic rock plates in the prior art.

[0008] Based on the above-mentioned purpose, the present invention provides a soft-light skin-feel glaze, a soft-light skin-feel ceramic rock plate with a digital three-dimensional effect, and a preparation method thereof.

[0009] A soft-gloss skin-feeling glaze, comprising a soft-gloss base glaze and a soft-gloss top glaze;

[0010] The soft gloss base glaze is prepared by mixing the following raw materials in parts by weight: 45-50 parts of potassium feldspar, 8-12 parts of kaolin, 4-6 parts of sodium feldspar, 2-4 parts of calcined alumina, 2-3 parts of calcined talc, 2-4 parts of dolomite, 3-5 parts of calcined kaolin, 10-15 parts of iodine, 30-35 parts of ethylene glycol butyl ether acetate, 2-5 parts of sodium lauryl sulfate, and 1-2 parts of triethanolamine;

[0011] The soft gloss glaze is obtained by mixing the following raw materials in parts by mass: 40-45 parts of potassium feldspar, 5-15 parts of sodium feldspar, 8-12 parts of kaolin, 10-15 parts of quartz, 10-15 parts of calcined alumina, 2-4 parts of wollastonite and 4-6 parts of calcined talc, 30-35 parts of ethylene glycol butyl ether acetate, 2-5 parts of sodium lauryl sulfate and 1-2 parts of triethanolamine.

[0012] A soft-light skin-feeling ceramic rock plate with a digital three-dimensional effect, comprising a blank and a soft-light skin-feeling glaze;

[0013] The blank is obtained by mixing the following raw materials in parts by weight: 40-50 parts of potassium feldspar, 4-8 parts of talc, 20-30 parts of kaolin, 5-10 parts of raw ore mud, 4-6 parts of wollastonite and 5-10 parts of toughening composition;

[0014] The toughening composition is obtained by mixing a reinforcing agent, lignin, hydroxypropyl methylcellulose and sodium polyacrylate in a mass ratio of 10-15:5-8:3-5:5-8;

[0015] The reinforcing agent is prepared from octamethylcyclotetrasiloxane, gamma-methacryloxypropyltrimethoxysilane, butyl acrylate and hydroxyethyl acrylate.

[0016] Preferably, the preparation method of the enhancer is as follows:

[0017] Step A1. Disperse dodecylbenzenesulfonic acid and octylphenol polyoxyethylene ether in deionized water, then add octamethylcyclotetrasiloxane and γ-methacryloxypropyltrimethoxysilane, stir at 60-65 ° C for 6-8 hours, and then cool to room temperature to obtain a pretreatment solution;

[0018] Step A2. Adjust the pH value of the pretreatment liquid to 8-10 with sodium hydroxide solution, raise the temperature to 70-80°C, add butyl acrylate and hydroxyethyl acrylate, and then add potassium persulfate aqueous solution. After reacting at 70-80°C for 3-6 hours, cool to room temperature, add calcium chloride aqueous solution, filter, wash, and dry to obtain an enhancer.

[0019] Preferably, the mass ratio of dodecylbenzenesulfonic acid, octylphenol polyoxyethylene ether, deionized water, octamethylcyclotetrasiloxane and γ-methacryloxypropyltrimethoxysilane in step A1 is 0.05-0.1:0.05-0.1:100-120:41-45:3-5.

[0020] Preferably, the mass ratio of the pretreatment liquid, butyl acrylate, hydroxyethyl acrylate, potassium persulfate aqueous solution and calcium chloride aqueous solution in step A2 is 55-60:31-35:13-18:1-3:25-30;

[0021] The mass fraction of the potassium persulfate aqueous solution in step A2 is 10%-15%;

[0022] The mass fraction of the calcium chloride aqueous solution in step A2 is 10%-15%.

[0023] A method for preparing a soft-light skin-feeling ceramic rock plate with a digital three-dimensional effect comprises the following steps:

[0024] Step B1. Potassium feldspar, talc, kaolin, raw ore mud, wollastonite and toughening composition are added, processed by ball milling equipment, and placed in a slurry tank for aging for 24-32 hours to obtain a slurry;

[0025] Step B2. spray drying the slurry to obtain slurry particles;

[0026] Step B3. After dry pressing the slurry particles, heating and drying, casting, soot blowing, and water spraying are performed to obtain a green body;

[0027] Step B4. After applying a soft base glaze on the surface of the blank, inkjet printing is performed on the surface with the soft base glaze, and then a soft top glaze is applied on the surface. The surface is fired under a nitrogen atmosphere to obtain a soft skin-feel glaze and a soft skin-feel ceramic rock plate with a digital three-dimensional effect.

[0028] Preferably, the particle size after ball milling in step B1 is 200-300 mesh.

[0029] Preferably, the air inlet temperature in the spray drying pulverizing in step B2 is 350-400°C, and the air outlet temperature is 70-75°C.

[0030] Preferably, the pressing pressure in the dry pressing molding in step B3 is 370-400 kg / cm 2 ;

[0031] The soft gloss base glaze in step B4 is applied by pouring glaze, and the amount of soft gloss base glaze applied is 240-260g / m 2 ;

[0032] The soft gloss glaze in step B4 is applied by pouring glaze, and the amount of soft gloss glaze applied is 650-700g / m 2 .

[0033] Preferably, the temperature in the sintering treatment in step B4 is:

[0034] From room temperature to 500℃, the heating rate is 30-40℃ / min;

[0035] From 500℃ to 850℃, the heating rate is 20-40℃ / min;

[0036] From 850℃ to 1100℃, the heating rate is 10-20℃ / min, and the temperature is kept at 1100℃ for 8-12min.

[0037] Beneficial effects of the present invention:

[0038] The formulas of the blank, soft-gloss base glaze and soft-gloss top glaze in the present invention all belong to clay minerals with good plasticity. At the same time, the toughening composition is added to the blank, which can greatly enhance the strength and toughness of the ceramic rock slab blank. The toughening composition has a certain adhesiveness and can form a bridge between the ceramic particles, thereby enhancing the bonding force between the particles. It has good thickening properties and can increase the viscosity of the ceramic slurry, so that the ceramic particles in the slurry are evenly dispersed and effective bonding is formed between the particles. During the drying process of the blank, this bonding effect helps to maintain the relative position of the particles, reduce the movement and agglomeration of the particles, thereby forming a more uniform and dense microstructure and improving the toughness of the ceramic rock slab. The present invention also effectively eliminates stress during the firing process through step-by-step temperature increase firing, improves the firing qualification rate, and reduces cracking, and has broad application prospects. DETAILED DESCRIPTION

[0039] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to specific embodiments.

[0040] The sources and properties of some of the raw materials used in the present invention are as follows:

[0041] Octamethylcyclotetrasiloxane was purchased from Jiangxi Lanxing Xinghuo Silicone Co., Ltd.; γ-methacryloxypropyltrimethoxysilane was purchased from Chengdu Kelon Chemical Reagent Factory; butyl acrylate was purchased from Shandong Langcheng Chemical Co., Ltd.; and hydroxyethyl acrylate was purchased from Liaoning Kelon Fine Chemical Co., Ltd.

[0042] Example 1: A soft-gloss skin-feeling glaze, comprising the following preparation steps:

[0043] S1. Potassium feldspar 45g, kaolin 8g, sodium feldspar 4g, calcined alumina 2g, calcined talc 2g, dolomite 2g, calcined kaolin 3g, iodine 10g, ethylene glycol butyl ether acetate 30g, sodium lauryl sulfate 2g and triethanolamine 1g were mixed to obtain a soft base glaze;

[0044] S2. Potassium feldspar 40g, sodium feldspar 5g, kaolin 8g, quartz 10g, calcined alumina 10g, wollastonite 2g and calcined talc 4g, ethylene glycol butyl ether acetate 30g, sodium lauryl sulfate 2g and triethanolamine 1g were mixed to obtain a soft glaze;

[0045] S3.Soft skin-feel glaze consists of soft base glaze and soft top glaze.

[0046] Example 2: A soft-gloss skin-feeling glaze, comprising the following preparation steps:

[0047] S1. Potassium feldspar 47g, kaolin 10g, sodium feldspar 5g, calcined alumina 3g, calcined talc 2.5g, dolomite 3g, calcined kaolin 4g, iodine 12g, ethylene glycol butyl ether acetate 32g, sodium lauryl sulfate 3g and triethanolamine 1.5g were mixed to obtain a soft base glaze;

[0048] S2. Potassium feldspar 42g, sodium feldspar 10g, kaolin 10g, quartz 12g, calcined alumina 12g, wollastonite 3g and calcined talc 5g, ethylene glycol butyl ether acetate 32g, sodium lauryl sulfate 3g and triethanolamine 1.5g were mixed to obtain a soft glaze;

[0049] S3.Soft skin-feel glaze consists of soft base glaze and soft top glaze.

[0050] Example 3: A soft-gloss skin-feeling glaze, comprising the following preparation steps:

[0051] S1. Potassium feldspar 48g, kaolin 11g, sodium feldspar 5.5g, calcined alumina 3.5g, calcined talc 2.8g, dolomite 3.5g, calcined kaolin 4.5g, iodine 13g, ethylene glycol butyl ether acetate 33g, sodium lauryl sulfate 4g and triethanolamine 1.8g were mixed to obtain a soft base glaze;

[0052] S2. Potassium feldspar 43g, sodium feldspar 12g, kaolin 11g, quartz 13g, calcined alumina 13g, wollastonite 3.5g and calcined talc 5.5g, ethylene glycol butyl ether acetate 33g, sodium lauryl sulfate 4g and triethanolamine 1.8g were mixed to obtain a soft glaze;

[0053] S3.Soft skin-feel glaze consists of soft base glaze and soft top glaze.

[0054] Example 4: A soft-gloss skin-feeling glaze, comprising the following preparation steps:

[0055] S1. Potassium feldspar 50g, kaolin 12g, sodium feldspar 6g, calcined alumina 4g, calcined talc 3g, dolomite 4g, calcined kaolin 5g, iodine 15g, ethylene glycol butyl ether acetate 35g, sodium lauryl sulfate 5g and triethanolamine 2g were mixed to obtain a soft base glaze;

[0056] S2. Potassium feldspar 45g, sodium feldspar 15g, kaolin 12g, quartz 15g, calcined alumina 15g, wollastonite 4g and calcined talc 6g, ethylene glycol butyl ether acetate 35g, sodium lauryl sulfate 5g and triethanolamine 2g were mixed to obtain a soft glaze;

[0057] S3.Soft skin-feel glaze consists of soft base glaze and soft top glaze.

[0058] Example 5: A method for preparing a soft-light skin-feeling ceramic rock plate with a digital three-dimensional effect, comprising the following steps:

[0059] S1. 0.05 g of dodecylbenzenesulfonic acid and 0.05 g of octylphenol polyoxyethylene ether were dispersed in 100 g of deionized water, and then 41 g of octamethylcyclotetrasiloxane and 3 g of γ-methacryloxypropyltrimethoxysilane were added. The mixture was stirred at 60 ° C for 6 h and then cooled to room temperature to obtain a pretreatment solution.

[0060] S2. The pretreatment solution was adjusted to pH 8 with 55g of sodium hydroxide solution, heated to 70°C, 31g of butyl acrylate and 13g of hydroxyethyl acrylate were added, followed by 1g of a 10% aqueous solution of potassium persulfate. The reaction was allowed to proceed at 70°C for 3h, and then cooled to room temperature. 25g of a 10% aqueous solution of calcium chloride was added, filtered, washed, and dried to obtain an enhancer.

[0061] S3. 10g of reinforcing agent, 5g of lignin, 3g of hydroxypropyl methylcellulose and 5g of sodium polyacrylate were mixed to obtain a toughening composition;

[0062] S4. The potassium feldspar 40g, talc 4g, kaolin 20g, raw ore mud 5g, wollastonite 4g and toughening composition 5g were mixed to obtain a blank;

[0063] S5. Potassium feldspar, talc, kaolin, raw ore mud, wollastonite and toughening composition were fed, processed by ball milling equipment, and placed in a slurry tank for aging for 24h to obtain a slurry, wherein the particle size after ball milling was 200 mesh;

[0064] S6. The slurry is spray dried to obtain slurry particles, wherein the inlet air temperature in the spray drying process is 350°C and the outlet air temperature is 70°C;

[0065] S7. After the slurry particles are dry-pressed and dried, the blank is thrown, soot is blown, and water is sprayed to obtain a blank, wherein the pressing pressure of the dry pressing is 370kg / cm 2 ;

[0066] S8. After applying the soft-light base glaze prepared in Example 1 on the surface of the body, inkjet printing is performed on the surface on which the soft-light base glaze is applied, and then the soft-light top glaze prepared in Example 1 is applied on the surface, and the surface is fired to obtain a soft-light skin-feeling glaze and a soft-light skin-feeling ceramic rock plate with a digital three-dimensional effect, wherein the soft-light base glaze is applied by pouring glaze, and the applied amount is 240g / m 2 ; The soft gloss glaze is applied by pouring glaze, and the application amount is 650g / m 2The temperature during the sintering treatment is: from room temperature to 500°C, the heating rate is 30°C / min; from 500°C to 850°C, the heating rate is 20°C / min; from 850°C to 1100°C, the heating rate is 10°C / min, and the temperature is kept at 1100°C for 8 minutes.

[0067] Example 6: A method for preparing a soft-light skin-feeling ceramic rock plate with a digital three-dimensional effect, comprising the following steps:

[0068] S1. 0.07 g of dodecylbenzenesulfonic acid and 0.07 g of octylphenol polyoxyethylene ether were dispersed in 110 g of deionized water, and then 43 g of octamethylcyclotetrasiloxane and 4 g of γ-methacryloxypropyltrimethoxysilane were added. The mixture was stirred at 62 ° C for 7 h and then cooled to room temperature to obtain a pretreatment solution.

[0069] S2. The pretreatment solution was adjusted to pH 9 with 57g of sodium hydroxide solution, heated to 75 ° C, 33g of butyl acrylate and 15g of hydroxyethyl acrylate were added, and then 2g of 12% potassium persulfate aqueous solution was added. After the reaction was allowed to react for 4h at 75 ° C, the mixture was cooled to room temperature, and 27g of 12% calcium chloride aqueous solution was added, filtered, washed, and dried to obtain an enhancer;

[0070] S3. 12g of reinforcing agent, 6g of lignin, 4g of hydroxypropyl methylcellulose and 6g of sodium polyacrylate were mixed to obtain a toughening composition;

[0071] S4. The potassium feldspar 45g, talc 6g, kaolin 25g, raw ore mud 7g, wollastonite 5g and toughening composition 7g were mixed to obtain a blank;

[0072] S5. Potassium feldspar, talc, kaolin, raw ore mud, wollastonite and toughening composition were fed, processed using ball milling equipment, and placed into the slurry tank for aging for 28h to obtain a slurry, wherein the particle size after ball milling was 250 mesh;

[0073] S6. The slurry is spray dried to obtain slurry particles, wherein the inlet air temperature in the spray drying process is 370°C and the outlet air temperature is 72°C;

[0074] S7. The slurry particles are dry pressed by a belt-type frameless press and then heated and dried, thrown, blown, and sprayed with water to obtain a green body, wherein the pressing pressure of the dry pressing is 380kg / cm 2 ;

[0075] S8. After applying the soft-gloss base glaze prepared in Example 2 on the surface of the blank, inkjet printing is performed on the surface on which the soft-gloss base glaze is applied, and then the soft-gloss top glaze prepared in Example 2 is applied on the surface, and the surface is fired to obtain a soft-gloss skin-feeling glaze and a soft-gloss skin-feeling ceramic rock plate with a digital three-dimensional effect, wherein the soft-gloss base glaze is applied by pouring glaze, and the applied amount is 250g / m 2 The soft gloss glaze is applied by pouring glaze, and the application amount is 670g / m 2 The temperature during the sintering treatment is: from room temperature to 500°C, the heating rate is 34°C / min; from 500°C to 850°C, the heating rate is 30°C / min; from 850°C to 1100°C, the heating rate is 14°C / min, and the temperature is kept at 1100°C for 10 minutes.

[0076] Example 7: A method for preparing a soft-light skin-feeling ceramic rock plate with a digital three-dimensional effect, comprising the following steps:

[0077] S1. 0.08 g of dodecylbenzenesulfonic acid and 0.08 g of octylphenol polyoxyethylene ether were dispersed in 115 g of deionized water, and then 44 g of octamethylcyclotetrasiloxane and 4.5 g of γ-methacryloyloxypropyltrimethoxysilane were added. The mixture was stirred at 63 ° C for 7.5 h and then cooled to room temperature to obtain a pre-treated solution.

[0078] S2. The pretreatment solution was adjusted to pH 9 with 58g of sodium hydroxide solution, heated to 78 ° C, 34g of butyl acrylate and 16g of hydroxyethyl acrylate were added, and then 2.5g of a 13% aqueous solution of potassium persulfate was added. After the reaction was allowed to react at 78 ° C for 5h, the mixture was cooled to room temperature, and 28g of a 13% aqueous solution of calcium chloride was added, filtered, washed, and dried to obtain an enhancer;

[0079] S3. 13g of reinforcing agent, 7g of lignin, 4.5g of hydroxypropyl methylcellulose and 7g of sodium polyacrylate were mixed to obtain a toughening composition;

[0080] S4. The potassium feldspar 48g, talc 7g, kaolin 28g, raw ore mud 8g, wollastonite 5.5g and toughening composition 8g were mixed to obtain a blank;

[0081] S5. Potassium feldspar, talc, kaolin, raw ore mud, wollastonite and toughening composition were fed, processed using ball milling equipment, and placed in a slurry tank for aging for 30h to obtain a slurry, wherein the particle size after ball milling was 280 mesh;

[0082] S6. The slurry is spray dried to obtain slurry particles, wherein the inlet air temperature in the spray drying process is 380°C and the outlet air temperature is 73°C;

[0083] S7. After dry pressing the slurry particles, they are heated and dried, thrown, blown, and sprayed with water to obtain a green body, wherein the pressing pressure of the dry pressing is 390kg / cm 2 ;

[0084] S8. After applying the soft-gloss base glaze prepared in Example 3 on the surface of the body, inkjet printing is performed on the surface on which the soft-gloss base glaze is applied, and then the soft-gloss top glaze prepared in Example 3 is applied on the surface, and the surface is fired to obtain a soft-gloss skin-feeling glaze and a soft-gloss skin-feeling ceramic rock plate with a digital three-dimensional effect, wherein the soft-gloss base glaze is applied by pouring glaze, and the applied amount is 255g / m 2 The soft gloss glaze is applied by pouring glaze, and the application amount is 680g / m 2 The temperature during the sintering treatment is: from room temperature to 500℃, the heating rate is 36℃ / min; from 500℃ to 850℃, the heating rate is 35℃ / min; from 850℃ to 1100℃, the heating rate is 16℃ / min, and the temperature is kept at 1100℃ for 11 minutes.

[0085] Example 8: A method for preparing a soft-light skin-feeling ceramic rock plate with a digital three-dimensional effect, comprising the following steps:

[0086] S1. 0.1 g of dodecylbenzenesulfonic acid and 0.1 g of octylphenol polyoxyethylene ether were dispersed in 120 g of deionized water, and then 45 g of octamethylcyclotetrasiloxane and 5 g of γ-methacryloxypropyltrimethoxysilane were added. The mixture was stirred at 65 ° C for 8 h and then cooled to room temperature to obtain a pre-treated solution.

[0087] S2. The pretreatment solution was adjusted to pH 10 with 60g of sodium hydroxide solution, heated to 80°C, 35g of butyl acrylate and 18g of hydroxyethyl acrylate were added, and then 3g of a 15% aqueous solution of potassium persulfate was added. After the reaction was allowed to react for 6h at 80°C, the mixture was cooled to room temperature and 30g of a 15% aqueous solution of calcium chloride was added, filtered, washed, and dried to obtain an enhancer;

[0088] S3. 15g of reinforcing agent, 8g of lignin, 5g of hydroxypropyl methylcellulose and 8g of sodium polyacrylate were mixed to obtain a toughening composition;

[0089] S4. The potassium feldspar 50g, talc 8g, kaolin 30g, raw ore mud 10g, wollastonite 6g and toughening composition 10g were mixed to obtain a blank;

[0090] S5. Potassium feldspar, talc, kaolin, raw ore mud, wollastonite and toughening composition were fed, processed by ball milling equipment, and placed into the slurry tank for aging for 32h to obtain a slurry, wherein the particle size after ball milling was 300 mesh;

[0091] S6. The slurry is spray dried to obtain slurry particles, wherein the inlet air temperature in the spray drying process is 400°C and the outlet air temperature is 75°C;

[0092] S7. After the slurry particles are dry-pressed and dried, the blank is thrown, soot is blown, and water is sprayed to obtain a blank, wherein the pressing pressure of the dry pressing is 400kg / cm 2 ;

[0093] S8. After applying the soft-light base glaze prepared in Example 4 on the surface of the blank, inkjet printing is performed on the surface on which the soft-light base glaze is applied, and then the soft-light top glaze prepared in Example 4 is applied on the surface, and the surface is fired to obtain a soft-light skin-feeling glaze and a soft-light skin-feeling ceramic rock plate with a digital three-dimensional effect, wherein the soft-light base glaze is applied by pouring glaze, and the applied amount is 260g / m 2 ; The soft gloss glaze is applied by pouring glaze, and the application amount is 700g / m 2 The temperature during the sintering treatment is: from room temperature to 500°C, the heating rate is 40°C / min; from 500°C to 850°C, the heating rate is 40°C / min; from 850°C to 1100°C, the heating rate is 20°C / min, and the temperature is kept at 1100°C for 12 minutes.

[0094] Comparative Example 1:

[0095] Compared with Example 1, this comparative example does not add an enhancer during the preparation process of the soft-light skin-feel ceramic rock plate. The remaining steps and parameters are the same and will not be repeated in this comparative example. Finally, a soft-light skin-feel ceramic rock plate is obtained.

[0096] Comparative Example 2:

[0097] Compared with Example 1, this comparative example did not add a toughening composition during the preparation process of the soft-light skin-feel ceramic rock plate. The remaining steps and parameters are the same and will not be repeated in this comparative example. Finally, a soft-light skin-feel ceramic rock plate is obtained.

[0098] Comparative Example 3:

[0099] Compared with Example 1, this comparative example only replaces "41g octamethylcyclotetrasiloxane and 3g γ-methacryloxypropyltrimethoxysilane" with "41g octamethylcyclotetrasiloxane and 20g γ-methacryloxypropyltrimethoxysilane". The remaining steps and parameters are the same and will not be repeated in this comparative example. Finally, a soft-light skin-feeling ceramic rock plate is obtained.

[0100] Comparative Example 4:

[0101] Compared with Example 1, this comparative example only replaces "100g of ethylene glycol butyl ether acetate" with "100g of water", and the remaining steps and parameters are the same. This comparative example will not be repeated, and finally a soft-light skin-feel ceramic rock plate is obtained.

[0102] Comparative Example 5:

[0103] Compared with Example 1, this comparative example only replaces "the temperature in the firing treatment is: from room temperature to 500°C, the heating rate is 30°C / min; from 500°C to 850°C, the heating rate is 20°C / min; from 850°C to 1100°C, the heating rate is 10°C / min, and keeping warm at 1100°C for 8 minutes" with "the temperature in the firing treatment is: from room temperature to 1100°C, the heating rate is 30°C / min, and keeping warm at 1100°C for 8 minutes". The remaining steps and parameters are the same and will not be repeated in this comparative example. Finally, a soft skin-feeling ceramic rock plate is obtained.

[0104] Performance testing:

[0105] Bending strength determination:

[0106] With reference to the test standard GB / T4741-1999 "Test method for flexural strength of ceramic materials", the ceramic rock slabs prepared in Examples 4 to 8 and Comparative Examples 1 to 5 were cut into specimens with a length of 30 mm, a width of 5 mm, and a thickness of 3 mm. The surface of the specimens was polished smooth and placed on the support device of a three-point bending tester. The loading pressure head was located at the midpoint directly above the specimen. Pressure was applied to the specimen at a constant rate, and the maximum fracture load borne by the specimen when it broke was recorded. The flexural strength of the ceramic rock slabs was calculated using the formula. The measured results are shown in Table 1.

[0107] Calculation formula for flexural strength:

[0108] Where σ is the bending strength, in MPa; F is the maximum breaking load, in N; L is the support point spacing, in mm; b is the specimen width, in mm; h is the specimen thickness, in mm.

[0109] Determination of processing fracture rate:

[0110] Cutting processing breakage rate: Take 50 pieces of ceramic rock slabs prepared in Examples 4 to 8 and Comparative Examples 1 to 5 respectively, and use an electric saw cutting machine to cut through the edges (within 1 / 3 of the side length) and the center (center line) of the ceramic rock slabs respectively.

[0111] If cracks or fracture lines other than the cutting lines are produced after cutting, it is considered a crack. If no visible cracks are produced after cutting, the modulus of rupture of the ceramic rock slab after cutting is measured. If the modulus of rupture changes to less than 90% of the original modulus of rupture, it is considered a crack; otherwise, it is considered not a crack. The measured results are shown in Table 1.

[0112] Engraving processing cracking rate: Take 50 ceramic rock slabs prepared in Examples 4 to 8 and Comparative Examples 1 to 5 respectively, and use a CNC water jet to engrave the central area of ​​the ceramic rock slab to engrave an annular hole with a depth of 5 mm, an inner diameter of 495 mm, and an outer diameter of 500 mm.

[0113] If the ceramic slab breaks during or after engraving, it is recorded as broken. If no visible cracks appear after engraving, the modulus of rupture of the ceramic slab after engraving is measured. If the modulus of rupture changes by less than 80% of the original modulus of rupture, it is considered broken. Otherwise, it is considered not broken. The measured results are shown in Table 1.

[0114] Qualified rate determination:

[0115] Drying qualification rate:

[0116] Take 500 pieces of the green bodies prepared in Examples 4 to 8 and Comparative Examples 1 to 5 and dry them. After drying, if the green bodies are broken or have small cracks on the edges and corners, they are considered unqualified; otherwise, they are considered qualified.

[0117] In addition, after drying, 20 qualified green bodies were selected and the side curvature and center curvature of the green bodies were measured with reference to the test standard GB3810.2-2016 "Test Methods for Ceramic Tiles Part 2". The results are shown in Table 2.

[0118] Firing qualification rate:

[0119] The qualified green body after drying is fired.

[0120] After firing, if there is a break or crack on the corners, or if there is obvious warping visible to the naked eye, it is considered unqualified; otherwise it is considered qualified;

[0121] After firing, 20 qualified ceramic slabs were selected and the edge curvature and center curvature were measured according to the test standard GB3810.2-2016 "Test Methods for Ceramic Tiles Part 2". The results are shown in Table 2.

[0122] Table 1 Statistics of bending strength, cutting cracking rate and engraving cracking rate

[0123] project Bending strength / MPa Cutting process fracture rate / % Carving cracking rate / % Example 5 43.8 1 4 Example 6 47.1 2 4 Example 7 41.5 1 4 Example 8 42.3 1 6 Comparative Example 1 31.8 5 34 Comparative Example 2 36.4 10 32 Comparative Example 3 29.6 16 27 Comparative Example 4 40.7 24 38 Comparative Example 5 40.2 25 40

[0124] Table 2 Statistics of drying and firing pass rates

[0125]

[0126]

[0127] Data Analysis:

[0128] As can be seen from Table 1, the soft light skin-feeling glaze and the soft light skin-feeling ceramic rock plate with digital three-dimensional effect prepared by the present invention have higher toughness, higher bending strength, and are not easy to break;

[0129] This may be because the formulas of the blank, soft-gloss base glaze and soft-gloss surface glaze in the present invention are all clay minerals with good plasticity. At the same time, the toughening composition is added to the blank, which can greatly enhance the strength and toughness of the ceramic rock slab. The toughening composition has a certain adhesiveness and can form a bridge between the ceramic particles, thereby enhancing the bonding force between the particles. It has good thickening properties and can increase the viscosity of the ceramic slurry, so that the ceramic particles in the slurry are evenly dispersed and form an effective bond between the particles. During the drying process of the blank, this bonding effect helps to maintain the relative position of the particles, reduce the movement and agglomeration of the particles, thereby forming a more uniform and dense microstructure and improving the toughness of the ceramic rock slab. The present invention also effectively eliminates stress during the firing process through step-by-step temperature increase, improves the firing qualification rate, and reduces cracking.

[0130] The toughening composition in the billet primarily enhances billet performance through its role in billet forming and drying. During the drying process, the water in the billet gradually evaporates, causing the billet to shrink in volume and prone to defects such as cracks. The toughening composition forms a network structure between the billet particles, acting as a bridge and support, improving the billet's drying strength and reducing cracking during the drying process. Although the toughening composition decomposes during high-temperature firing, before decomposition, it helps to tightly bind and evenly distribute the particles in the billet. After decomposition, the billet has formed a relatively stable and compact particle stacking structure, which, to a certain extent, improves the strength and toughness of the rock slab.

[0131] The organic solvents in the soft base glaze and soft top glaze will gradually and slowly evaporate as the firing temperature gradient increases. Since the ceramic body and glaze have certain pores and channels, these volatile substances can be discharged in an orderly manner along these paths, and will not form a large pressure difference inside the rock slab, will not cause obvious holes in the rock slab, and will not affect the mechanical properties of the ceramic rock slab.

[0132] In Comparative Example 1, since no reinforcing agent was added during the preparation of the ceramic rock plate, it can be seen from Tables 1 and 2 that the flexural strength of the prepared ceramic rock plate decreased, the toughness was low, and it was easy to crack. This may be because the reinforcing agent not only has the excellent adhesion and film-forming properties of polyacrylate, but also has the heat resistance and weather resistance of silicone. The reinforcing agent is a core-shell structure polymer with an organic silicon polymer as the core and a polyacrylate as the shell. It can solve the problem of phase separation in the polymerization process caused by the difference in polarity between the organic silicon monomer and the acrylate monomer. The reinforcing agent can improve the toughness of the ceramic rock plate.

[0133] In Comparative Example 2, since no toughening composition was added during the preparation of the ceramic rock slab, it can be seen from Tables 1 and 2 that the flexural strength of the prepared ceramic rock slab decreased, the toughness was low, and it was prone to cracking. This may be because the reinforcing agent, lignin, hydroxypropyl methylcellulose, and sodium polyacrylate in the toughening composition are mixed in a specific ratio, which can improve the toughness of the ceramic rock slab. The toughening composition has a certain adhesiveness and can form a bridge between ceramic particles, thereby enhancing the bonding force between particles. It has good thickening properties and can increase the viscosity of the ceramic slurry, so that the ceramic particles in the slurry are evenly dispersed and form an effective bond between the particles. During the drying and sintering process of the green body, this bonding effect helps to maintain the relative position of the particles, reduce the movement and agglomeration of the particles, thereby forming a more uniform and dense microstructure and improving the toughness of the ceramic rock slab.

[0134] Comparative Example 3: Since "41g octamethylcyclotetrasiloxane and 3g γ-methacryloxypropyltrimethoxysilane" is replaced by "41g octamethylcyclotetrasiloxane and 20g γ-methacryloxypropyltrimethoxysilane", it can be seen from Tables 1 and 2 that the flexural strength and toughness of the ceramic rock plate are reduced. This may be because the content of γ-methacryloxypropyltrimethoxysilane is too high. On the one hand, γ-methacryloxypropyltrimethoxysilane will undergo hydrolysis and self-polymerization reaction, resulting in the formation of a cross-linked structure, which destroys the copolymerization reaction with octamethylcyclotetrasiloxane and cannot play the role of the flexibility of the silicone polymer chain segment; on the other hand, the increase in the amount of γ-methacryloxypropyltrimethoxysilane reduces the number of silicon-oxygen bonds on the polysiloxane chain, reduces the flexibility of the polysiloxane chain, and thus leads to a decrease in toughness;

[0135] In Comparative Example 4, since "100g of ethylene glycol butyl ether acetate" was replaced with "100g of water", it can be seen from Tables 1 and 2 that the flexural strength and toughness of the ceramic rock plate decreased. This may be because ethylene glycol butyl ether acetate is an organic solvent and has good solubility for the film-forming substances in the base glaze, which can help form a continuous, uniform, and dense film. Water, as a solvent, has limited solubility for some film-forming substances, which may lead to defects in the film formation process, such as discontinuous films and pinholes, affecting the protective effect of the base glaze on the ceramic rock plate, making the rock plate more susceptible to damage such as cracks when subjected to external forces, and reducing toughness.

[0136] In Comparative Example 5, since the gradient heating in the firing step is changed to one-step heating, it can be seen from Tables 1 and 2 that the flexural strength of the ceramic rock plate decreases and the toughness decreases. This may be because the gradient heating allows the ceramic rock plate blank to gradually adapt to thermal changes at different temperature stages, allowing the internal stress to be slowly released and adjusted. In the case of one-step heating, the blank is heated rapidly in a short period of time. Due to the difference in heat conduction in different parts, a large temperature gradient will be generated, which will lead to thermal stress concentration. These concentrated thermal stresses may form defects such as microcracks inside the blank, seriously reducing the toughness of the rock plate and making it more likely to break when subjected to external forces.

[0137] The present invention is intended to cover all such substitutions, modifications and variations that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A soft light skin-feel glaze, characterized in that: Including soft gloss base glaze and soft gloss top glaze; The soft gloss base glaze is prepared by mixing the following raw materials in parts by weight: 45-50 parts of potassium feldspar, 8-12 parts of kaolin, 4-6 parts of sodium feldspar, 2-4 parts of calcined alumina, 2-3 parts of calcined talc, 2-4 parts of dolomite, 3-5 parts of calcined kaolin, 10-15 parts of iodine, 30-35 parts of ethylene glycol butyl ether acetate, 2-5 parts of sodium lauryl sulfate, and 1-2 parts of triethanolamine; The soft gloss glaze is obtained by mixing the following raw materials in parts by mass: 40-45 parts of potassium feldspar, 5-15 parts of sodium feldspar, 8-12 parts of kaolin, 10-15 parts of quartz, 10-15 parts of calcined alumina, 2-4 parts of wollastonite and 4-6 parts of calcined talc, 30-35 parts of ethylene glycol butyl ether acetate, 2-5 parts of sodium lauryl sulfate and 1-2 parts of triethanolamine.

2. A soft-light skin-feeling ceramic rock plate with a digital three-dimensional effect prepared from the soft-light skin-feeling glaze according to claim 1, characterized in that: The soft light skin feeling ceramic rock plate with digital three-dimensional effect includes a blank and a soft light skin feeling glaze; The blank is obtained by mixing the following raw materials in parts by weight: 40-50 parts of potassium feldspar, 4-8 parts of talc, 20-30 parts of kaolin, 5-10 parts of raw ore mud, 4-6 parts of wollastonite and 5-10 parts of toughening composition; The toughening composition is obtained by mixing a reinforcing agent, lignin, hydroxypropyl methylcellulose and sodium polyacrylate in a mass ratio of 10-15:5-8:3-5:5-8; The preparation method of the enhancer is as follows: Step A1. Disperse dodecylbenzenesulfonic acid and octylphenol polyoxyethylene ether in deionized water, then add octamethylcyclotetrasiloxane and γ-methacryloxypropyltrimethoxysilane, stir at 60-65 ° C for 6-8 hours, and then cool to room temperature to obtain a pretreatment solution; Step A2. Adjust the pH value of the pretreatment liquid to 8-10 with sodium hydroxide solution, raise the temperature to 70-80°C, add butyl acrylate and hydroxyethyl acrylate, and then add potassium persulfate aqueous solution. After reacting at 70-80°C for 3-6 hours, cool to room temperature, add calcium chloride aqueous solution, filter, wash, and dry to obtain an enhancer.

3. The soft light skin-feeling ceramic rock plate with digital three-dimensional effect according to claim 2 is characterized in that: The mass ratio of dodecylbenzenesulfonic acid, octylphenol polyoxyethylene ether, deionized water, octamethylcyclotetrasiloxane and γ-methacryloxypropyltrimethoxysilane in step A1 is 0.05-0.1:0.05-0.1:100-120:41-45:3-5.

4. The soft light skin-feeling ceramic rock plate with digital three-dimensional effect according to claim 2 is characterized in that: The mass ratio of the pretreatment solution, butyl acrylate, hydroxyethyl acrylate, potassium persulfate aqueous solution and calcium chloride aqueous solution in step A2 is 55-60:31-35:13-18:1-3:25-30; The mass fraction of the potassium persulfate aqueous solution in step A2 is 10%-15%; The mass fraction of the calcium chloride aqueous solution in step A2 is 10%-15%.

5. The method for preparing a soft light skin-feeling ceramic rock plate with digital three-dimensional effect according to any one of claims 2 to 4, characterized in that: The following steps are involved: Step B1. Potassium feldspar, talc, kaolin, raw ore mud, wollastonite and toughening composition are added, processed by ball milling equipment, and placed in a slurry tank for aging for 24-32 hours to obtain a slurry; Step B2. spray drying the slurry to obtain slurry particles; Step B3. After dry pressing the slurry particles, heating and drying, casting, soot blowing, and water spraying are performed to obtain a green body; Step B4. After applying a soft-gloss base glaze on the surface of the blank, inkjet printing is performed on the surface with the soft-gloss base glaze, and then a soft-gloss top glaze is applied on the surface. The surface is fired in a nitrogen atmosphere to obtain a soft-gloss skin-feel ceramic rock plate with a digital three-dimensional effect.

6. The method for preparing the soft light skin-feeling ceramic rock plate with digital three-dimensional effect according to claim 5 is characterized in that: The particle size after ball milling in step B1 is 200-300 mesh.

7. The method for preparing the soft light skin-feeling ceramic rock plate with digital three-dimensional effect according to claim 5 is characterized in that: The inlet air temperature in the spray drying powder production in step B2 is 350-400°C, and the outlet air temperature is 70-75°C.

8. The method for preparing the soft light skin-feeling ceramic rock plate with digital three-dimensional effect according to claim 5 is characterized in that: The pressing pressure in the dry pressing molding in step B3 is 370-400kg / cm 2 ; The soft gloss base glaze in step B4 is applied by pouring glaze, and the amount of soft gloss base glaze applied is 240-260g / m 2 ; The soft gloss glaze in step B4 is applied by pouring glaze, and the amount of soft gloss glaze applied is 650-700g / m 2 .

9. The method for preparing the soft light skin-feeling ceramic rock plate with digital three-dimensional effect according to claim 5 is characterized in that: The temperature during the sintering treatment in step B4 is: From room temperature to 500℃, the heating rate is 30-40℃ / min; From 500℃ to 850℃, the heating rate is 20-40℃ / min; From 850℃ to 1100℃, the heating rate is 10-20℃ / min, and the temperature is kept at 1100℃ for 8-12min.

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