Travertine dry granular glaze and preparation method thereof
By introducing alumina-silica microspheres coated with talc into travertine dry granule glaze, the problem of easy cracking of the glaze layer under stress concentration is solved, the flexural strength is improved, the service life is extended, and the construction and maintenance difficulty is reduced.
Patent Information
- Application Number
- CN202511136027.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-14
- Publication Date
- 2025-10-28
- Estimated Expiration
- 2045-08-14
AI Technical Summary
Travertine dry granular glaze is prone to micro-cracks or breakage due to stress concentration during transportation, handling and installation, which increases the difficulty of construction and maintenance and limits its popularity in the mass market.
Alumina-silica microspheres coated with talc are introduced into solid raw materials to improve the flexural strength of the glaze by dispersing the impact force in stages, and to prevent crack propagation by utilizing the buffering effect of the talc layer.
It effectively improves the flexural strength of travertine dry granule glaze, extends the service life of the glaze layer, and reduces the difficulty of construction and maintenance.
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Figure SMS_7
Abstract
Description
Technical Field
[0001] This invention belongs to the field of ceramic technology and relates to a dry granular travertine glaze and its preparation method. Background Technology
[0002] Travertine dry-granule glaze is a ceramic surface decoration material that imitates the texture of natural travertine. Its core feature is the use of the granular texture and layering variations of the dry-granule glaze to mimic the porous structure and mineral crystallization effect of natural travertine. It is widely used in building walls and floors, furniture countertops, etc. However, because dry-granule glaze is processed from various mineral raw materials, the compatibility and particle size distribution between different raw materials are difficult to match perfectly. This results in a dense porous structure inside the glaze layer after firing. When imitating the texture of natural travertine, this structural characteristic is further amplified. This makes it prone to micro-cracks or even breakage due to stress concentration during transportation, handling, and installation, increasing the difficulty of construction and maintenance and limiting its popularity in the mass market. Summary of the Invention
[0003] The purpose of this invention is to provide a dry granular travertine glaze and its preparation method. This invention introduces alumina-silica microspheres coated with talc into solid raw materials. When the glaze surface is subjected to external impact, the alumina-silica microspheres coated with talc disperse the impact force from the outside to the inside, giving the dry granular glaze good flexural strength and effectively resisting external impact, thereby effectively extending the service life of the glaze layer.
[0004] The purpose of the present invention can be achieved through the following technical solutions: A travertine granule glaze, wherein the raw materials of the travertine granule glaze, by percentage, include 58-62 wt% solid raw materials, 0.3-0.5 wt% hydroxyethyl cellulose, 0.16-0.2 wt% sodium tripolyphosphate, and the balance being water.
[0005] Furthermore, the solid raw materials, by percentage, include 30-37 wt% quartz sand, 18-26 wt% potassium feldspar, 15-18 wt% kaolin, 5-10 wt% alumina-silica microspheres coated with talc, 3-7 wt% calcium oxide, 2-4 wt% potassium oxide, and the balance zinc oxide.
[0006] Furthermore, the solid raw material is obtained by a method comprising the following steps: X1. Mix quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide, and zinc oxide, and ball mill at 200-300 rpm for 3-5 hours. Then pass the mixture through a 40-60 mesh sieve to obtain a premix. X2. Mix the premixed material and the alumina-silicon microspheres coated with talc evenly to obtain a solid raw material.
[0007] Furthermore, the method for preparing the alumina-silica microspheres coated with talc includes the following steps: Y1. Mix talc powder, silica sol, and sodium hexametaphosphate evenly to obtain talc slurry; Y2. The silica sol was spray-dried and calcined to obtain silica microspheres; Y3. The silicon microspheres and isopropanol were ultrasonically mixed and then aluminum sol was added dropwise. The mixture was stirred, centrifuged and washed, and then calcined to obtain alumina-silicon microspheres. Y4. Mix alumina-silicon microspheres, 3-aminopropyltriethoxysilane, and ethanol solution to obtain coupled alumina-silicon microspheres. Y5. The talc slurry is evenly sprayed onto the coupled alumina-silicon microspheres and calcined to obtain alumina-silicon microspheres with talc coating on the surface.
[0008] Further, the talc powder in step Y1 is obtained by ball milling talc at 250-350 rpm for 1.5-2.5 hours and then passing it through a 60-80 mesh sieve; the mass ratio of the talc powder, silica sol, and sodium hexametaphosphate is 1:0.1-0.14:0.01-0.03.
[0009] Furthermore, the calcination mentioned in step Y2 refers to calcination at 950-1050℃ for 1.5-2.5 hours in an argon atmosphere.
[0010] Further, in step Y3, the mass ratio of microspheres, isopropanol, and aluminum sol is 1:9.6-10.8:0.3-0.5; the ultrasonic mixing refers to setting the ultrasonic frequency to 30-50kHz, the ultrasonic frequency to 200-400W, and ultrasonication for 25-35 minutes; the stirring refers to stirring at 58-62℃ and 300-400rpm for 1.5-2.5 hours; and the calcination refers to calcining at 485-515℃ for 1-2 hours.
[0011] Further, in step Y4, the mass ratio of alumina-silica microspheres, 3-aminopropyltriethoxysilane, and ethanol solution is 1:0.04-0.06:10-11; the ethanol solution is an 88-92 wt% ethanol solution; the mixing refers to adjusting the pH to 5-6 and stirring at 60°C for 2-3 hours.
[0012] Further, the mass ratio of the alumina-silica microspheres and talc slurry after coupling treatment in step Y5 is 1:1.1-1.3; the calcination refers to calcination at 585-615℃ for 1-1.2h.
[0013] Furthermore, the preparation method of the travertine dry granule glaze includes the following steps: Z1. Mix solid raw materials, hydroxyethyl cellulose, sodium tripolyphosphate and water, and stir at 450-550 rpm for 1-2 hours to obtain dry granule glaze slurry. Z2. Using a spray glazing process, the dry granule glaze slurry is applied at a specific gravity of 1.1-1.3 g / ml. Spray 30-40g onto the surface of the brick blank, then calcine at 1140-1200℃ for 30-40 minutes.
[0014] The beneficial effects of this invention are: This invention provides a travertine granular glaze, in which alumina-silica microspheres coated with talc are added. The talc-coated microspheres have better compatibility with other solid raw materials, and their lubricating properties help them disperse evenly, thereby effectively reducing interface defects in the granular glaze. When the substrate with the granular glaze is subjected to external impact, the talc coating forms a layered structure with different orientations. Energy diffuses along this layered structure, thus effectively buffering the impact. If cracks are generated during the stress process, the cracks will be hindered as they extend to the talc layer, thereby changing the direction of crack extension and preventing further deepening and expansion. At this time, the remaining external force is further transmitted to the alumina layer and silica microspheres step by step through the flexible siloxane chain of 3-aminopropyltriethoxysilane, avoiding excessive deformation or breakage under external impact, which would result in large fracture points and exacerbate the cracking of the glaze layer, thus effectively extending the service life of the glaze layer. Detailed Implementation
[0015] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with embodiments, is provided below.
[0016] Example 1 A travertine granule glaze, wherein the raw materials of the travertine granule glaze, by percentage, comprise 58 wt% solid raw materials, 0.3 wt% hydroxyethyl cellulose, 0.16 wt% sodium tripolyphosphate, and the balance being water.
[0017] The solid raw materials, by percentage, include 30wt% quartz sand, 18wt% potassium feldspar, 15wt% kaolin, 5wt% alumina-silica microspheres coated with talc, 3wt% calcium oxide, 2-4wt% potassium oxide, and the balance zinc oxide.
[0018] The solid raw material is obtained by a method comprising the following steps: X1. Mix quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide, and zinc oxide, ball mill at 200 rpm for 3 hours, and then pass through a 40-mesh sieve to obtain a premix. X2. Mix the premixed material and the alumina-silicon microspheres coated with talc evenly to obtain a solid raw material.
[0019] The method for preparing the talc-coated alumina-silica microspheres includes the following steps: Y1. Mix talc powder, silica sol, and sodium hexametaphosphate evenly to obtain talc slurry; Y2. The silica sol was spray-dried and calcined to obtain silica microspheres; Y3. The silicon microspheres and isopropanol were ultrasonically mixed and then aluminum sol was added dropwise. The mixture was stirred, centrifuged and washed, and then calcined to obtain alumina-silicon microspheres. Y4. Mix alumina-silicon microspheres, 3-aminopropyltriethoxysilane, and ethanol solution to obtain coupled alumina-silicon microspheres. Y5. The talc slurry is evenly sprayed onto the coupled alumina-silicon microspheres and calcined to obtain alumina-silicon microspheres with talc coating on the surface.
[0020] The talc powder mentioned in step Y1 is obtained by ball milling talc at 250 rpm for 1.5 hours and then passing it through a 60-mesh sieve; the mass ratio of talc powder, silica sol, and sodium hexametaphosphate is 1:0.1:0.01.
[0021] The calcination mentioned in step Y2 refers to calcination at 950°C for 1.5 hours in an argon atmosphere.
[0022] The mass ratio of microspheres, isopropanol, and aluminum sol in step Y3 is 1:9.6:0.3; ultrasonic mixing refers to setting the ultrasonic frequency to 30kHz and 200W for 25 minutes; stirring refers to stirring at 300rpm at 58℃ for 1.5 hours; calcination refers to calcining at 485℃ for 1 hour.
[0023] In step Y4, the mass ratio of alumina-silica microspheres, 3-aminopropyltriethoxysilane, and ethanol solution is 1:0.04:10; the ethanol solution is 88wt% ethanol solution; mixing refers to adjusting the pH to 5 and stirring at 60°C for 2 hours.
[0024] The mass ratio of alumina-silica microspheres to talc slurry after coupling treatment in step Y5 is 1:1.1; calcination refers to calcination at 585℃ for 1 hour.
[0025] The preparation method of the travertine dry granule glaze includes the following steps: Z1. Mix solid raw materials, hydroxyethyl cellulose, sodium tripolyphosphate and water, and stir at 450 rpm for 1 hour to obtain dry granule glaze slurry; Z2. Using a spray glazing process, the dry granule glaze slurry is applied at a specific gravity of 1.1 g / ml. Spray 30g onto the surface of the brick blank and then calcine at 1140℃ for 30 minutes.
[0026] Example 2 A travertine granule glaze, wherein the raw materials of the travertine granule glaze, by percentage, comprise 59 wt% solid raw materials, 0.35 wt% hydroxyethyl cellulose, 0.17 wt% sodium tripolyphosphate, and the balance being water.
[0027] The solid raw materials, by percentage, include 32 wt% quartz sand, 20 wt% potassium feldspar, 16 wt% kaolin, 6.5 wt% alumina-silica microspheres coated with talc, 4 wt% calcium oxide, 2.5 wt% potassium oxide, and the balance zinc oxide.
[0028] The solid raw material is obtained by a method comprising the following steps: X1. Mix quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide and zinc oxide, ball mill at 200 rpm for 3.5 hours, and then pass through a 40-mesh sieve to obtain a premix. X2. Mix the premixed material and the alumina-silicon microspheres coated with talc evenly to obtain a solid raw material.
[0029] The method for preparing the talc-coated alumina-silica microspheres includes the following steps: Y1. Mix talc powder, silica sol, and sodium hexametaphosphate evenly to obtain talc slurry; Y2. The silica sol was spray-dried and calcined to obtain silica microspheres; Y3. The silicon microspheres and isopropanol were ultrasonically mixed and then aluminum sol was added dropwise. The mixture was stirred, centrifuged and washed, and then calcined to obtain alumina-silicon microspheres. Y4. Mix alumina-silicon microspheres, 3-aminopropyltriethoxysilane, and ethanol solution to obtain coupled alumina-silicon microspheres. Y5. The talc slurry is evenly sprayed onto the coupled alumina-silicon microspheres and calcined to obtain alumina-silicon microspheres with talc coating on the surface.
[0030] The talc powder mentioned in step Y1 is obtained by ball milling talc at 250 rpm for 1.5 hours and then passing it through a 60-mesh sieve; the mass ratio of talc powder, silica sol, and sodium hexametaphosphate is 1:0.1:0.01.
[0031] The calcination mentioned in step Y2 refers to calcination at 9580℃ for 1.7h in an argon atmosphere.
[0032] The mass ratio of microspheres, isopropanol, and aluminum sol in step Y3 is 1:9.9:0.35; ultrasonic mixing refers to setting the ultrasonic frequency to 30kHz and 200W for 28 minutes; stirring refers to stirring at 300rpm at 59℃ for 1.7 hours; calcination refers to calcining at 495℃ for 1.2 hours.
[0033] In step Y4, the mass ratio of alumina-silica microspheres, 3-aminopropyltriethoxysilane, and ethanol solution is 1:0.04:10.3; the ethanol solution is 89wt% ethanol solution; mixing refers to adjusting the pH to 5.2 and stirring at 60℃ for 2.3h.
[0034] The mass ratio of alumina-silica microspheres to talc slurry after coupling treatment in step Y5 is 1:1.15; calcination refers to calcination at 595℃ for 1 hour.
[0035] The preparation method of the travertine dry granule glaze includes the following steps: Z1. Mix solid raw materials, hydroxyethyl cellulose, sodium tripolyphosphate and water, and stir at 450 rpm for 1.2 h to obtain dry granule glaze slurry; Z2. Using a spray glazing process, the dry granule glaze slurry is applied at a specific gravity of 1.15 g / ml. Spray 32g onto the surface of the brick blank and then calcine at 1160℃ for 32min.
[0036] Example 3 A travertine granule glaze, wherein the raw materials of the travertine granule glaze, by percentage, comprise 60 wt% solid raw materials, 0.4 wt% hydroxyethyl cellulose, 0.18 wt% sodium tripolyphosphate, and the balance being water.
[0037] The solid raw material comprises, by percentage, 33.5 wt% quartz sand, 22 wt% potassium feldspar, 16.5 wt% kaolin, 7.5 wt% alumina-silica microspheres coated with talc, 5 wt% calcium oxide, 3 wt% potassium oxide, and the balance zinc oxide.
[0038] The solid raw material is obtained by a method comprising the following steps: X1. Mix quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide, and zinc oxide, ball mill at 250 rpm for 4 hours, and then pass through a 50-mesh sieve to obtain a premix. X2. Mix the premixed material and the alumina-silicon microspheres coated with talc evenly to obtain a solid raw material.
[0039] The method for preparing the talc-coated alumina-silica microspheres includes the following steps: Y1. Mix talc powder, silica sol, and sodium hexametaphosphate evenly to obtain talc slurry; Y2. The silica sol was spray-dried and calcined to obtain silica microspheres; Y3. The silicon microspheres and isopropanol were ultrasonically mixed and then aluminum sol was added dropwise. The mixture was stirred, centrifuged and washed, and then calcined to obtain alumina-silicon microspheres. Y4. Mix alumina-silicon microspheres, 3-aminopropyltriethoxysilane, and ethanol solution to obtain coupled alumina-silicon microspheres. Y5. The talc slurry is evenly sprayed onto the coupled alumina-silicon microspheres and calcined to obtain alumina-silicon microspheres with talc coating on the surface.
[0040] The talc powder mentioned in step Y1 is obtained by ball milling talc at 300 rpm for 2 hours and then passing it through a 70-mesh sieve; the mass ratio of talc powder, silica sol, and sodium hexametaphosphate is 1:0.12:0.02.
[0041] The calcination mentioned in step Y2 refers to calcination at 1000℃ for 2 hours under an argon atmosphere.
[0042] The mass ratio of microspheres, isopropanol, and aluminum sol in step Y3 is 1:10.2:0.4; ultrasonic mixing refers to setting the ultrasonic frequency to 40kHz and 300W for 30 minutes; stirring refers to stirring at 350rpm at 60℃ for 2 hours; calcination refers to calcining at 500℃ for 1.5 hours.
[0043] In step Y4, the mass ratio of alumina-silica microspheres, 3-aminopropyltriethoxysilane, and ethanol solution is 1:0.05:10.5; the ethanol solution is 90wt% ethanol solution; mixing refers to adjusting the pH to 5.5 and stirring at 60℃ for 2.5h.
[0044] The mass ratio of alumina-silica microspheres to talc slurry after coupling treatment in step Y5 is 1:1.2; calcination refers to calcination at 600℃ for 1.1h.
[0045] The preparation method of the travertine dry granule glaze includes the following steps: Z1. Mix solid raw materials, hydroxyethyl cellulose, sodium tripolyphosphate and water, and stir at 500 rpm for 1.5 h to obtain dry granule glaze slurry; Z2. Using a spray glazing process, the dry granule glaze slurry is applied at a specific gravity of 1.2 g / ml. Spray 35g onto the surface of the brick blank and then calcine at 1170℃ for 35 minutes.
[0046] Example 4 A travertine granule glaze, wherein the raw materials of the travertine granule glaze, by percentage, comprise 61 wt% solid raw materials, 0.45 wt% hydroxyethyl cellulose, 0.19 wt% sodium tripolyphosphate, and the balance being water.
[0047] The solid raw material comprises, by percentage, 35 wt% quartz sand, 24 wt% potassium feldspar, 17 wt% kaolin, 8.5 wt% alumina-silica microspheres coated with talc, 6 wt% calcium oxide, 3.5 wt% potassium oxide, and the balance zinc oxide.
[0048] The solid raw material is obtained by a method comprising the following steps: X1. Mix quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide and zinc oxide, ball mill at 300 rpm for 4.5 hours, and then pass through a 60-mesh sieve to obtain a premix. X2. Mix the premixed material and the alumina-silicon microspheres coated with talc evenly to obtain a solid raw material.
[0049] The method for preparing the talc-coated alumina-silica microspheres includes the following steps: Y1. Mix talc powder, silica sol, and sodium hexametaphosphate evenly to obtain talc slurry; Y2. The silica sol was spray-dried and calcined to obtain silica microspheres; Y3. The silicon microspheres and isopropanol were ultrasonically mixed and then aluminum sol was added dropwise. The mixture was stirred, centrifuged and washed, and then calcined to obtain alumina-silicon microspheres. Y4. Mix alumina-silicon microspheres, 3-aminopropyltriethoxysilane, and ethanol solution to obtain coupled alumina-silicon microspheres. Y5. The talc slurry is evenly sprayed onto the coupled alumina-silicon microspheres and calcined to obtain alumina-silicon microspheres with talc coating on the surface.
[0050] The talc powder mentioned in step Y1 is obtained by ball milling talc at 350 rpm for 2.2 hours and then passing it through an 80-mesh sieve; the mass ratio of talc powder, silica sol, and sodium hexametaphosphate is 1:0.13:0.03.
[0051] The calcination mentioned in step Y2 refers to calcination at 1020℃ for 2.3 hours in an argon atmosphere.
[0052] The mass ratio of microspheres, isopropanol, and aluminum sol in step Y3 is 1:10.5:0.45; ultrasonic mixing refers to setting the ultrasonic frequency to 50kHz and 400W for 32 minutes; stirring refers to stirring at 400rpm at 61℃ for 2.2 hours; calcination refers to calcining at 510℃ for 1.8 hours.
[0053] In step Y4, the mass ratio of alumina-silica microspheres, 3-aminopropyltriethoxysilane, and ethanol solution is 1:0.06:10.7; the ethanol solution is 91wt% ethanol solution; mixing refers to adjusting the pH to 5.8 and stirring at 60°C for 2.8 hours.
[0054] The mass ratio of alumina-silica microspheres to talc slurry after coupling treatment in step Y5 is 1:1.25; calcination refers to calcination at 610℃ for 1.2h.
[0055] The preparation method of the travertine dry granule glaze includes the following steps: Z1. Mix solid raw materials, hydroxyethyl cellulose, sodium tripolyphosphate and water, and stir at 550 rpm for 2 hours to obtain dry granule glaze slurry. Z2. Using a spray glazing process, the dry granule glaze slurry is applied at a specific gravity of 1.25 g / ml. Spray 37g onto the surface of the brick blank and then calcine at 1180℃ for 38 minutes.
[0056] Example 5 A travertine granule glaze, wherein the raw materials of the travertine granule glaze, by percentage, comprise 62 wt% solid raw materials, 0.5 wt% hydroxyethyl cellulose, 0.2 wt% sodium tripolyphosphate, and the balance being water.
[0057] The solid raw materials, by percentage, include 37 wt% quartz sand, 26 wt% potassium feldspar, 18 wt% kaolin, 10 wt% alumina-silica microspheres coated with talc, 7 wt% calcium oxide, 4 wt% potassium oxide, and the balance zinc oxide.
[0058] The solid raw material is obtained by a method comprising the following steps: X1. Mix quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide, and zinc oxide, ball mill at 300 rpm for 5 hours, and then pass through a 60-mesh sieve to obtain a premix. X2. Mix the premixed material and the alumina-silicon microspheres coated with talc evenly to obtain a solid raw material.
[0059] The method for preparing the talc-coated alumina-silica microspheres includes the following steps: Y1. Mix talc powder, silica sol, and sodium hexametaphosphate evenly to obtain talc slurry; Y2. The silica sol was spray-dried and calcined to obtain silica microspheres; Y3. The silicon microspheres and isopropanol were ultrasonically mixed and then aluminum sol was added dropwise. The mixture was stirred, centrifuged and washed, and then calcined to obtain alumina-silicon microspheres. Y4. Mix alumina-silicon microspheres, 3-aminopropyltriethoxysilane, and ethanol solution to obtain coupled alumina-silicon microspheres. Y5. The talc slurry is evenly sprayed onto the coupled alumina-silicon microspheres and calcined to obtain alumina-silicon microspheres with talc coating on the surface.
[0060] The talc powder mentioned in step Y1 is obtained by ball milling talc at 350 rpm for 2.5 hours and then passing it through an 80-mesh sieve; the mass ratio of talc powder, silica sol, and sodium hexametaphosphate is 1:0.14:0.03.
[0061] The calcination mentioned in step Y2 refers to calcination at 1050℃ for 2.5 hours in an argon atmosphere.
[0062] The mass ratio of microspheres, isopropanol, and aluminum sol in step Y3 is 1:10.8:0.5; ultrasonic mixing refers to setting the ultrasonic frequency to 50kHz and 400W for 35 minutes; stirring refers to stirring at 400rpm at 62℃ for 2.5 hours; calcination refers to calcining at 515℃ for 2 hours.
[0063] In step Y4, the mass ratio of alumina-silica microspheres, 3-aminopropyltriethoxysilane, and ethanol solution is 1:0.06:11; the ethanol solution is 92wt% ethanol solution; mixing refers to adjusting the pH to 6 and stirring at 60°C for 3 hours.
[0064] The mass ratio of alumina-silica microspheres to talc slurry after coupling treatment in step Y5 is 1:1.3; calcination refers to calcination at 615℃ for 1.2h.
[0065] The preparation method of the travertine dry granule glaze includes the following steps: Z1. Mix solid raw materials, hydroxyethyl cellulose, sodium tripolyphosphate and water, and stir at 550 rpm for 2 hours to obtain dry granule glaze slurry. Z2. Using a spray glazing process, the dry granule glaze slurry is applied at a specific gravity of 1.3 g / ml. Spray 40g onto the surface of the brick blank and then calcine at 1200℃ for 40 minutes.
[0066] Example 6 Based on Example 3, the alumina-silicon microspheres coated with talc were removed and replaced with an equal weight of talc powder, which was obtained by ball milling talc at 300 rpm for 2 hours and then passing it through a 70-mesh sieve.
[0067] Comparative Example 1 Based on Example 3, keeping other conditions unchanged, the preparation method of alumina-silica microspheres coated with talc was changed to include the following steps: Y1. Mix talc powder, silica sol, and sodium hexametaphosphate evenly to obtain talc slurry; Y2. The silica sol was spray-dried and calcined to obtain silica microspheres; Y3. The silicon microspheres and isopropanol were ultrasonically mixed and then aluminum sol was added dropwise. The mixture was stirred, centrifuged and washed, and then calcined to obtain alumina-silicon microspheres. Y4. The talc slurry is evenly sprayed onto the alumina-silicon microspheres and calcined to obtain alumina-silicon microspheres with talc coating on the surface.
[0068] Comparative Example 2 Based on Example 3, keeping other conditions unchanged, the alumina-silicon microspheres with talc coating were replaced with alumina-silicon microspheres. The preparation method of the alumina-silicon microspheres includes the following steps: Y1. The silica sol was spray-dried and calcined to obtain silica microspheres; Y2. The silicon microspheres and isopropanol are ultrasonically mixed and then aluminum sol is added dropwise. The mixture is stirred, centrifuged and washed, and then calcined to obtain alumina-silicon microspheres.
[0069] Comparative Example 3 Based on Example 3, keeping other conditions unchanged, the alumina-silicon microspheres with talc coating were replaced with alumina with talc coating. The preparation method of the alumina with talc coating includes the following steps: Y1. Mix talc powder, silica sol, and sodium hexametaphosphate evenly to obtain talc slurry; Y2. Mix aluminum oxide, 3-aminopropyltriethoxysilane, and ethanol solution to obtain coupled aluminum oxide; Y3. The talc slurry is evenly sprayed onto the coupled alumina and calcined to obtain alumina with talc coating.
[0070] Using the travertine dry granule glazes obtained in Examples 1-6 and Comparative Examples 1-3 as samples, the flexural strength of the samples was tested according to GB / T 4100-2015, and the test results are recorded in Table 1 below.
[0071] As shown in Table 1, the travertine dry granule glaze prepared by this invention has good flexural strength and can effectively resist external impact, thereby effectively extending the service life of the glaze layer.
[0072] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any indirect modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.
Claims
1. A travertine dry-granule glaze, characterized in that: The raw materials of the travertine dry granule glaze, by percentage, include 58-62 wt% solid raw materials, 0.3-0.5 wt% hydroxyethyl cellulose, 0.16-0.2 wt% sodium tripolyphosphate, and the balance being water.
2. The travertine dry-granule glaze according to claim 1, characterized in that: The solid raw materials, by percentage, include 30-37 wt% quartz sand, 18-26 wt% potassium feldspar, 15-18 wt% kaolin, 5-10 wt% alumina-silica microspheres coated with talc, 3-7 wt% calcium oxide, 2-4 wt% potassium oxide, and the balance zinc oxide.
3. The travertine dry-granule glaze according to claim 1, characterized in that: The solid raw material is obtained by a method comprising the following steps: X1. Mix quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide, and zinc oxide, and ball mill at 200-300 rpm for 3-5 hours. Then pass the mixture through a 40-60 mesh sieve to obtain a premix. X2. Mix the premixed material and the alumina-silicon microspheres coated with talc evenly to obtain a solid raw material.
4. The travertine dry-granule glaze according to claim 2, characterized in that: The method for preparing the talc-coated alumina-silica microspheres includes the following steps: Y1. Mix talc powder, silica sol, and sodium hexametaphosphate evenly to obtain talc slurry; Y2. The silica sol was spray-dried and calcined to obtain silica microspheres; Y3. The silicon microspheres and isopropanol were ultrasonically mixed and then aluminum sol was added dropwise. The mixture was stirred, centrifuged and washed, and then calcined to obtain alumina-silicon microspheres. Y4. Mix alumina-silicon microspheres, 3-aminopropyltriethoxysilane, and ethanol solution to obtain coupled alumina-silicon microspheres. Y5. The talc slurry is evenly sprayed onto the coupled alumina-silicon microspheres and calcined to obtain alumina-silicon microspheres with talc coating on the surface.
5. The travertine dry-granule glaze according to claim 4, characterized in that: The talc powder mentioned in step Y1 is obtained by ball milling talc at 250-350 rpm for 1.5-2.5 hours and then passing it through a 60-80 mesh sieve; the mass ratio of the talc powder, silica sol, and sodium hexametaphosphate is 1:0.1-0.14:0.01-0.
03.
6. The travertine dry-granule glaze according to claim 4, characterized in that: The calcination mentioned in step Y2 refers to calcination at 950-1050℃ for 1.5-2.5 hours in an argon atmosphere.
7. The travertine dry-granule glaze according to claim 4, characterized in that: The mass ratio of microspheres, isopropanol, and aluminum sol in step Y3 is 1:9.6-10.8:0.3-0.5; the ultrasonic mixing refers to setting the ultrasonic frequency to 30-50kHz, the ultrasonic frequency to 200-400W, and ultrasonication for 25-35 minutes; the stirring refers to stirring at 300-400rpm at 58-62℃ for 1.5-2.5 hours; the calcination refers to calcining at 485-515℃ for 1-2 hours.
8. The travertine dry-granule glaze according to claim 4, characterized in that: In step Y4, the mass ratio of alumina-silica microspheres, 3-aminopropyltriethoxysilane, and ethanol solution is 1:0.04-0.06:10-11; the ethanol solution is an 88-92 wt% ethanol solution; the mixing refers to adjusting the pH to 5-6 and stirring at 60°C for 2-3 hours.
9. A travertine dry-granule glaze according to claim 4, characterized in that: The mass ratio of alumina-silica microspheres to talc slurry after coupling treatment in step Y5 is 1:1.1-1.3; the calcination refers to calcination at 585-615℃ for 1-1.2h.
10. A method for preparing travertine dry granule glaze as described in any one of claims 1-9, characterized in that: The preparation method of the travertine dry granule glaze includes the following steps: Z1. Mix solid raw materials, hydroxyethyl cellulose, sodium tripolyphosphate and water, and stir at 450-550 rpm for 1-2 hours to obtain dry granule glaze slurry. Z2. Using a spray glazing process, the dry granule glaze slurry is applied at a specific gravity of 1.1-1.3 g / ml. Spray 30-40g onto the surface of the brick blank, then calcine at 1140-1200℃ for 30-40 minutes.
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