A hole stone dry granular glaze and a preparation method thereof

By introducing alumina-silica microspheres coated with talc into travertine dry granule glaze, the problem of easy cracking of the glaze under stress concentration was solved, and the high flexural strength and long service life of the glaze were achieved.

CN120841841BActive Publication Date: 2026-03-27FOSHAN TAOYING NEW MATERIAL CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-08-14
Publication Date
2026-03-27

AI Technical Summary

Technical Problem

Travertine dry granule glaze is prone to micro-cracks or fractures due to stress concentration during transportation, handling and installation, which affects construction and maintenance and limits its popularity in the mass market.

Method used

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 step by step. The buffering effect of the talc layer and the flexible chain of 3-aminopropyltriethoxysilane are used to transfer the external force, thus avoiding excessive deformation or breakage of the glaze.

Benefits of technology

It effectively improves the flexural strength of the glaze, extends its service life, and reduces the risk of cracking of the glaze under external impact.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application relates to a kind of hole stone dry granular glaze and its preparation method, belong to ceramic technical field.The present application provides a kind of hole stone dry granular glaze, raw material includes solid raw material, hydroxyethyl cellulose, sodium tripolyphosphate and water, by introducing the alumina-silicon microspheres of surface coating talc into solid raw material, when glaze surface bears external force impact, alumina-silicon microspheres of surface coating talc is gradually dispersed impact force from outside to inside, give dry granular glaze good flexural strength, can effectively resist external impact force, to effectively prolong the service life of glaze layer.
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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 during transportation, handling, and installation due to stress concentration. This increases the difficulty of construction and maintenance, 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 objective of this invention can be achieved through the following technical solutions:

[0005] 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.

[0006] 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.

[0007] Furthermore, the solid raw material is obtained by a method comprising the following steps:

[0008] 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.

[0009] X2. Mix the premixed material and the alumina-silicon microspheres coated with talc evenly to obtain a solid raw material.

[0010] Further, the preparation method of the surface-coated talc alumina-silica microspheres comprises the following steps:

[0011] Y1, talc powder, silica sol, sodium hexametaphosphate are uniformly mixed to obtain talc slurry;

[0012] Y2, the silica sol is spray dried and calcined to obtain silica microspheres;

[0013] Y3, the silica microspheres, isopropyl alcohol are ultrasonically mixed, then aluminum sol is added dropwise, stirred, centrifuged, washed, and calcined to obtain alumina-silica microspheres;

[0014] Y4, the alumina-silica microspheres, 3-aminopropyl triethoxysilane, and ethanol solution are mixed to obtain alumina-silica microspheres after coupling treatment;

[0015] Y5, the talc slurry is uniformly sprayed on the alumina-silica microspheres after coupling treatment, and calcined to obtain surface-coated talc alumina-silica microspheres.

[0016] Further, the talc powder in step Y1 is obtained by ball milling the talc at a speed of 250-350 rpm for 1.5-2.5 h, and then passing 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.

[0017] Further, the calcination in step Y2 refers to calcining at 950-1050℃ for 1.5-2.5 h under argon environment.

[0018] Further, the mass ratio of the microspheres, isopropyl alcohol, 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 30-50 kHz, the ultrasonic frequency to 200-400 W, and ultrasonic mixing for 25-35 min; the stirring refers to stirring at a speed of 300-400 rpm at 58-62℃ for 1.5-2.5 h; the calcination refers to calcining at 485-515℃ for 1-2 h.

[0019] Further, the mass ratio of the alumina-silica microspheres, 3-aminopropyl triethoxysilane, and ethanol solution in step Y4 is 1:0.04-0.06:10-11; the ethanol solution is 88-92 wt% ethanol solution; the mixing refers to adjusting the pH to 5-6 and stirring at 60℃ for 2-3 h.

[0020] Further, the mass ratio of the alumina-silica microspheres after coupling treatment and the talc slurry in step Y5 is 1:1.1-1.3; the calcination refers to calcining at 585-615℃ for 1-1.2 h.

[0021] Further, the preparation method of the hole stone dry granular glaze comprises the following steps:

[0022] Z1, after mixing the solid raw material, hydroxyethyl cellulose, sodium tripolyphosphate and water, stirring at a speed of 450-550 rpm for 1-2 h, to obtain a dry granular glaze slurry;

[0023] Z2, using the glaze spraying process, the dry granular glaze slurry is sprayed on the surface of the brick body at a specific gravity of 1.1-1.3 g / ml, / pan, 30-40 g of the dry granular glaze is sprayed on the surface of the brick body, and then calcined at 1140-1200 ℃ for 30-40 min.

[0024] The beneficial effects of the present application are:

[0025] The present application provides a hole stone dry granular glaze, in which alumina-silicon microspheres coated with talc on the surface are added. The compatibility between the microspheres coated with talc and other solid raw materials is better, and the lubricating property helps the uniform dispersion, thereby effectively reducing the interface defects in the dry granular glaze. When the substrate applied with the dry granular glaze is impacted by external force, the talc coated outside forms a layered structure with different directions, and the energy spreads along the layered structure, thereby effectively playing a buffering role. If a crack is generated during the force process, the crack will be hindered by the talc layer when it expands to the talc layer, thereby changing the expansion direction of the crack to prevent the crack from further deepening and expanding. At this time, the remaining external force further transmits to the alumina layer and the silicon microspheres in stages through the flexible silicon-oxygen chain of 3-aminopropyl triethoxysilane, avoiding excessive deformation or breaking under external impact, thereby appearing large cracking points, aggravating the rupture of the glaze layer, and effectively prolonging the service life of the glaze layer. DETAILED DESCRIPTION

[0026] In order to further illustrate the technical means and effects adopted by the present application to achieve the predetermined application purpose, the specific embodiments, structures, features and effects according to the present application are described in detail as follows in combination with examples.

[0027] Example 1

[0028] A hole stone dry granular glaze, the raw materials of the hole stone dry granular glaze include, by percentage, 58wt% solid raw material, 0.3wt% hydroxyethyl cellulose, 0.16wt% sodium tripolyphosphate and the balance of water.

[0029] The raw materials of the solid raw material include, by percentage, 30wt% quartz sand, 18wt% potassium feldspar, 15wt% kaolin, 5wt% alumina-silicon microspheres coated with talc on the surface, 3wt% calcium oxide, 2-4wt% potassium oxide and the balance of zinc oxide.

[0030] The solid raw material is obtained by a method comprising the following steps:

[0031] X1, quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide, zinc oxide were mixed, ball milled at 200 rpm for 3 h, and then sieved through a 40-mesh screen to obtain a premix;

[0032] X2, the premix and the alumina-silica microspheres coated with talc were mixed uniformly to obtain a solid raw material.

[0033] The preparation method of the alumina-silica microspheres coated with talc comprises the following steps:

[0034] Y1, talc powder, silica sol, and sodium hexametaphosphate were mixed uniformly to obtain a talc slurry;

[0035] Y2, the silica sol was spray dried and calcined to obtain silica microspheres;

[0036] Y3, the silica microspheres, isopropyl alcohol, and aluminum sol were ultrasonically mixed, and then the aluminum sol was added dropwise, stirred, centrifuged and washed, and calcined to obtain alumina-silica microspheres;

[0037] Y4, the alumina-silica microspheres, 3-aminopropyl triethoxysilane, and an ethanol solution were mixed to obtain alumina-silica microspheres after coupling treatment;

[0038] Y5, the talc slurry was uniformly sprayed on the alumina-silica microspheres after coupling treatment, and then calcined to obtain alumina-silica microspheres coated with talc.

[0039] The talc powder in step Y1 was obtained by ball milling talc at 250 rpm for 1.5 h and then sieving through a 60-mesh screen; the mass ratio of talc powder, silica sol, and sodium hexametaphosphate was 1:0.1:0.01.

[0040] The calcination in step Y2 refers to calcination at 950°C for 1.5 h under an argon atmosphere.

[0041] In step Y3, the mass ratio of microspheres, isopropyl alcohol, and aluminum sol was 1:9.6:0.3; ultrasonic mixing refers to setting the ultrasonic frequency to 30 kHz and the ultrasonic frequency to 200 W, and ultrasonic mixing for 25 min; stirring refers to stirring at 58°C at a rotation speed of 300 rpm for 1.5 h; and calcination refers to calcination at 485°C for 1 h.

[0042] In step Y4, the mass ratio of alumina-silica microspheres, 3-aminopropyl triethoxysilane, and an ethanol solution was 1:0.04:10; the ethanol solution was an 88 wt% ethanol solution; and mixing refers to adjusting the pH to 5 and stirring at 60°C for 2 h.

[0043] In step Y5, the mass ratio of alumina-silica microspheres after coupling treatment and talc slurry was 1:1.1; and calcination refers to calcination at 585°C for 1 h.

[0044] The preparation method of the hole stone dry granular glaze comprises the following steps:

[0045] Z1, after mixing the solid raw material, hydroxyethyl cellulose, sodium tripolyphosphate and water, stirring at a speed of 450 rpm for 1 h, a dry granular glaze slurry is obtained;

[0046] Z2, using the glaze spraying process, the dry granular glaze slurry is sprayed on the brick body surface at a specific gravity of 1.1 g / ml, 30 g per disc, and then calcined at 1140℃ for 30 min.

[0047] Example 2

[0048] A hole stone dry granular glaze, the raw materials of the hole stone dry granular glaze comprise, by percentage, 59wt% solid raw material, 0.35wt% hydroxyethyl cellulose, 0.17wt% sodium tripolyphosphate and the balance of water.

[0049] The raw materials of the solid raw material comprise, by percentage, 32wt% quartz sand, 20wt% potassium feldspar, 16wt% kaolin, 6.5wt% alumina-silicon microspheres coated with talc on the surface, 4wt% calcium oxide, 2.5wt% potassium oxide and the balance of zinc oxide.

[0050] The solid raw material is obtained by a method comprising the following steps:

[0051] X1, after mixing the quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide and zinc oxide, ball milling at a speed of 200 rpm for 3.5 h, and then passing through a 40 mesh sieve, a premix is obtained;

[0052] X2, uniformly mixing the premix and the alumina-silicon microspheres coated with talc on the surface to obtain the solid raw material.

[0053] The preparation method of the alumina-silicon microspheres coated with talc on the surface comprises the following steps:

[0054] Y1, uniformly mixing the talc powder, silica sol and sodium hexametaphosphate to obtain a talc slurry;

[0055] Y2, spray drying the silica sol, and calcining to obtain silica microspheres;

[0056] Y3, after ultrasonic mixing the silica microspheres and isopropyl alcohol, adding an aluminum sol dropwise, stirring, centrifugal washing, and calcining, alumina-silicon microspheres are obtained;

[0057] Y4, mixing the alumina-silicon microspheres, 3-aminopropyl triethoxysilane and an ethanol solution to obtain the alumina-silicon microspheres after coupling treatment;

[0058] Y5, uniformly spraying the talc slurry on the alumina-silicon microspheres after coupling treatment, and calcining to obtain the alumina-silicon microspheres coated with talc on the surface.

[0059] The talc powder in step Y1 is obtained by ball milling talc at 250 rpm for 1.5 h and then passing through a 60-mesh sieve; the mass ratio of talc powder, silica sol, and sodium hexametaphosphate is 1:0.1:0.01.

[0060] The calcination in step Y2 refers to calcination at 9580℃ for 1.7 h in an argon environment.

[0061] The mass ratio of microspheres, isopropyl alcohol, and aluminum sol in step Y3 is 1:9.9:0.35; the ultrasonic mixing refers to setting the ultrasonic frequency to 30 kHz, the ultrasonic frequency to 200 W, and the ultrasonic time to 28 min; the stirring refers to stirring at 59℃ at a rotation speed of 300 rpm for 1.7 h; the calcination refers to calcination at 495℃ for 1.2 h.

[0062] The mass ratio of alumina-silica microspheres, 3-aminopropyl triethoxysilane, and ethanol solution in step Y4 is 1:0.04:10.3; the ethanol solution is 89wt% ethanol solution; the mixing refers to adjusting the pH to 5.2 and stirring at 60℃ for 2.3 h.

[0063] The mass ratio of the alumina-silica microspheres after coupling treatment and the talc slurry in step Y5 is 1:1.15; the calcination refers to calcination at 595℃ for 1 h.

[0064] The preparation method of the hole stone dry granular glaze comprises the following steps:

[0065] Z1, after mixing the solid raw material, hydroxyethyl cellulose, sodium tripolyphosphate, and water, stirring at 450 rpm for 1.2 h, a dry granular glaze slurry is obtained;

[0066] Z2, using the glaze spraying process, the dry granular glaze slurry is sprayed on the surface of the brick body at a specific gravity of 1.15 g / ml, 32 g per disc, and then calcined at 1160℃ for 32 min.

[0067] Example 3

[0068] A hole stone dry granular glaze, the raw materials of the hole stone dry granular glaze comprise, by percentage, 60wt% solid raw material, 0.4wt% hydroxyethyl cellulose, 0.18wt% sodium tripolyphosphate, and the balance of water.

[0069] The raw materials of the solid raw material comprise, by percentage, 33.5wt% quartz sand, 22wt% potassium feldspar, 16.5wt% kaolin, 7.5wt% alumina-silica microspheres coated with talc on the surface, 5wt% calcium oxide, 3wt% potassium oxide, and the balance of zinc oxide.

[0070] The solid raw material is obtained by a method comprising the following steps:

[0071] X1, quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide, zinc oxide were mixed, ball milled at 250 rpm for 4 h, and then sieved through a 50 mesh screen to obtain a premix;

[0072] X2, the premix and the alumina-silica microspheres coated with talc were mixed uniformly to obtain a solid raw material.

[0073] The preparation method of the alumina-silica microspheres coated with talc comprises the following steps:

[0074] Y1, talc powder, silica sol, and sodium hexametaphosphate were mixed uniformly to obtain a talc slurry;

[0075] Y2, the silica sol was spray dried and calcined to obtain silica microspheres;

[0076] Y3, the silica microspheres, isopropyl alcohol, and aluminum sol were ultrasonically mixed, and then the aluminum sol was added dropwise, stirred, centrifuged and washed, and calcined to obtain alumina-silica microspheres;

[0077] Y4, the alumina-silica microspheres, 3-aminopropyl triethoxysilane, and an ethanol solution were mixed to obtain alumina-silica microspheres after coupling treatment;

[0078] Y5, the talc slurry was uniformly sprayed on the alumina-silica microspheres after coupling treatment, and then calcined to obtain alumina-silica microspheres coated with talc.

[0079] The talc powder in step Y1 was obtained by ball milling talc at 300 rpm for 2 h and then sieving through a 70 mesh screen; the mass ratio of talc powder, silica sol, and sodium hexametaphosphate was 1:0.12:0.02.

[0080] The calcination in step Y2 refers to calcination at 1000°C for 2 h under an argon atmosphere.

[0081] In step Y3, the mass ratio of microspheres, isopropyl alcohol, and aluminum sol was 1:10.2:0.4; ultrasonic mixing refers to setting the ultrasonic frequency to 40 kHz and the ultrasonic power to 300 W, and ultrasonic mixing for 30 min; stirring refers to stirring at 60°C at a rotation speed of 350 rpm for 2 h; and calcination refers to calcination at 500°C for 1.5 h.

[0082] In step Y4, the mass ratio of alumina-silica microspheres, 3-aminopropyl triethoxysilane, and an ethanol solution was 1:0.05:10.5; the ethanol solution was a 90 wt% ethanol solution; and mixing refers to adjusting the pH to 5.5 and stirring at 60°C for 2.5 h.

[0083] In step Y5, the mass ratio of alumina-silica microspheres after coupling treatment and talc slurry was 1:1.2; and calcination refers to calcination at 600°C for 1.1 h.

[0084] The preparation method of the dry granular hole stone glaze comprises the following steps:

[0085] Z1, after mixing the solid raw material, hydroxyethyl cellulose, sodium tripolyphosphate and water, stirring at a speed of 500 rpm for 1.5 h, a dry granular glaze slurry is obtained;

[0086] Z2, using the glazing process, the dry granular glaze slurry is sprayed on the surface of the brick body at a specific gravity of 1.2 g / ml, 35 g per disc, and then calcined at 1170℃ for 35 min.

[0087] Example 4

[0088] A dry granular hole stone glaze, the raw materials of the dry granular hole stone glaze comprise, by percentage, 61wt% solid raw material, 0.45wt% hydroxyethyl cellulose, 0.19wt% sodium tripolyphosphate and the balance of water.

[0089] The raw materials of the solid raw material comprise, by percentage, 35wt% quartz sand, 24wt% potassium feldspar, 17wt% kaolin, 8.5wt% alumina-silicon microspheres coated with talc on the surface, 6wt% calcium oxide, 3.5wt% potassium oxide and the balance of zinc oxide.

[0090] The solid raw material is obtained by a method comprising the following steps:

[0091] X1, after mixing the quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide and zinc oxide, ball milling at a speed of 300 rpm for 4.5 h, and then passing through a 60 mesh sieve, a premix is obtained;

[0092] X2, uniformly mixing the premix and the alumina-silicon microspheres coated with talc on the surface to obtain the solid raw material.

[0093] The preparation method of the alumina-silicon microspheres coated with talc on the surface comprises the following steps:

[0094] Y1, uniformly mixing the talc powder, silica sol and sodium hexametaphosphate to obtain a talc slurry;

[0095] Y2, spray drying the silica sol, calcining to obtain silica microspheres;

[0096] Y3, after ultrasonic mixing the silica microspheres and isopropyl alcohol, adding dropwise an aluminum sol, stirring, centrifugal washing, calcining to obtain alumina-silicon microspheres;

[0097] Y4, mixing the alumina-silicon microspheres, 3-aminopropyl triethoxysilane and ethanol solution to obtain the coupling-treated alumina-silicon microspheres;

[0098] Y5, the talc slurry is uniformly sprayed on the alumina-silica microspheres after coupling treatment, and calcination is performed to obtain alumina-silica microspheres coated with talc on the surface.

[0099] The talc powder in step Y1 is obtained by ball milling talc at a speed of 350 rpm for 2.2 h, and then passing through an 80-mesh sieve; the mass ratio of talc powder, silica sol, and sodium hexametaphosphate is 1:0.13:0.03.

[0100] The calcination in step Y2 refers to calcination at 1020℃ for 2.3 h in an argon environment.

[0101] The mass ratio of microspheres, isopropyl alcohol, and aluminum sol in step Y3 is 1:10.5:0.45; the ultrasonic mixing refers to setting the ultrasonic frequency to 50 kHz, the ultrasonic frequency to 400 W, and ultrasonic mixing for 32 min; the stirring refers to stirring at a speed of 400 rpm for 2.2 h at 61℃; and the calcination refers to calcination at 510℃ for 1.8 h.

[0102] The mass ratio of alumina-silica microspheres, 3-aminopropyl triethoxysilane, and ethanol solution in step Y4 is 1:0.06:10.7; the ethanol solution is a 91wt% ethanol solution; and the mixing refers to adjusting the pH to 5.8 and stirring at 60℃ for 2.8 h.

[0103] The mass ratio of alumina-silica microspheres after coupling treatment and talc slurry in step Y5 is 1:1.25; and the calcination refers to calcination at 610℃ for 1.2 h.

[0104] The preparation method of the hole stone dry granular glaze comprises the following steps:

[0105] Z1, after mixing the solid raw material, hydroxyethyl cellulose, sodium tripolyphosphate, and water, stirring is performed at a speed of 550 rpm for 2 h to obtain a dry granular glaze slurry;

[0106] Z2, the dry granular glaze slurry is sprayed on the brick body surface according to a specific gravity of 1.25 g / ml, 37 g per disc, and calcination is performed at 1180℃ for 38 min.

[0107] Example 5

[0108] A hole stone dry granular glaze, the raw materials of the hole stone dry granular glaze comprise, by percentage, 62wt% solid raw material, 0.5wt% hydroxyethyl cellulose, 0.2wt% sodium tripolyphosphate, and the balance of water.

[0109] The raw materials of the solid raw material comprise, by percentage, 37wt% quartz sand, 26wt% potassium feldspar, 18wt% kaolin, 10wt% alumina-silica microspheres coated with talc on the surface, 7wt% calcium oxide, 4wt% potassium oxide, and the balance of zinc oxide.

[0110] The solid raw material is obtained by a method comprising the following steps:

[0111] X1, quartz sand, potassium feldspar, kaolin, calcium oxide, potassium oxide, zinc oxide are mixed, ball-milled at a speed of 300 rpm for 5 h, and then sieved through a 60-mesh sieve to obtain a premix;

[0112] X2, the premix and the talc-coated alumina-silicon microspheres are uniformly mixed to obtain the solid raw material.

[0113] The preparation method of the talc-coated alumina-silicon microspheres comprises the following steps:

[0114] Y1, talc powder, silica sol, and sodium hexametaphosphate are uniformly mixed to obtain a talc slurry;

[0115] Y2, the silica sol is spray-dried and calcined to obtain silica microspheres;

[0116] Y3, the silica microspheres, isopropyl alcohol, and aluminum sol are ultrasonically mixed, and then the aluminum sol is added dropwise, stirred, centrifuged and washed, and calcined to obtain alumina-silicon microspheres;

[0117] Y4, the alumina-silicon microspheres, 3-aminopropyl triethoxysilane, and an ethanol solution are mixed to obtain alumina-silicon microspheres after coupling treatment;

[0118] Y5, the talc slurry is uniformly sprayed on the alumina-silicon microspheres after coupling treatment, and then calcined to obtain talc-coated alumina-silicon microspheres.

[0119] The talc powder in step Y1 is obtained by ball-milling talc at a speed of 350 rpm for 2.5 h and then sieving through an 80-mesh sieve; the mass ratio of talc powder, silica sol, and sodium hexametaphosphate is 1:0.14:0.03.

[0120] The calcination in step Y2 refers to calcination at 1050°C for 2.5 h under an argon atmosphere.

[0121] The mass ratio of the microspheres, isopropyl alcohol, and aluminum sol in step Y3 is 1:10.8:0.5; the ultrasonic mixing refers to setting the ultrasonic frequency to 50 kHz and the ultrasonic power to 400 W, and ultrasonic mixing for 35 min; the stirring refers to stirring at a speed of 400 rpm at 62°C for 2.5 h; and the calcination refers to calcination at 515°C for 2 h.

[0122] The mass ratio of the alumina-silicon microspheres, 3-aminopropyl triethoxysilane, and an ethanol solution in step Y4 is 1:0.06:11; the ethanol solution is a 92 wt% ethanol solution; and the mixing refers to adjusting the pH to 6 and stirring at 60°C for 3 h.

[0123] The mass ratio of the alumina-silicon microspheres and the talc slurry after the coupling treatment in step Y5 is 1:1.3; the calcination refers to calcination at 615°C for 1.2h.

[0124] The preparation method of the hole stone dry granular glaze comprises the following steps:

[0125] Z1, after mixing the solid raw materials, hydroxyethyl cellulose, sodium tripolyphosphate and water, stirring at a speed of 550 rpm for 2h, dry granular glaze slurry is obtained;

[0126] Z2, using the glaze spraying process, the dry granular glaze slurry is sprayed on the brick body surface at a specific gravity of 1.3g / ml, / pan, 40g of the dry granular glaze slurry is sprayed on the surface of the brick body, and then the brick body is calcined at 1200°C for 40min.

[0127] Example 6

[0128] On the basis of Example 3, the alumina-silicon microspheres coated with talc on the surface are replaced with talc powder of the same weight, and the talc powder is obtained by ball milling talc at a speed of 300 rpm for 2h and then passing through a 70 mesh sieve.

[0129] Comparative Example 1

[0130] On the basis of Example 3, the preparation method of the alumina-silicon microspheres coated with talc on the surface is changed to comprise the following steps:

[0131] Y1, talc powder, silica sol and sodium hexametaphosphate are mixed uniformly to obtain talc slurry;

[0132] Y2, the silica sol is spray dried and calcined to obtain silica microspheres;

[0133] Y3, the silica microspheres are mixed with isopropyl alcohol by ultrasonic, then aluminum sol is added dropwise, stirred, centrifuged and washed, and calcined to obtain alumina-silicon microspheres;

[0134] Y4, the talc slurry is uniformly sprayed on the alumina-silicon microspheres, and then calcined to obtain alumina-silicon microspheres coated with talc on the surface.

[0135] Comparative Example 2

[0136] On the basis of Example 3, the alumina-silicon microspheres coated with talc on the surface are changed to alumina-silicon microspheres, and the preparation method of the alumina-silicon microspheres comprises the following steps:

[0137] Y1, the silica sol is spray dried and calcined to obtain silica microspheres;

[0138] Y2, the silica microspheres are mixed with isopropyl alcohol by ultrasonic, then aluminum sol is added dropwise, stirred, centrifuged and washed, and calcined to obtain alumina-silicon microspheres.

[0139] Comparative Example 3

[0140] On the basis of Example 3, other conditions remain unchanged, the surface-coated talc alumina-silicon microspheres are changed to surface-coated talc alumina, the preparation method of the surface-coated talc alumina comprises the following steps:

[0141] Y1, talc powder, silica sol, sodium hexametaphosphate are uniformly mixed to obtain a talc slurry;

[0142] Y2, alumina, 3-aminopropyl triethoxysilane, ethanol solution are mixed to obtain the coupling-treated alumina;

[0143] Y3, the talc slurry is uniformly sprayed on the coupling-treated alumina, and calcination is performed to obtain the surface-coated talc alumina.

[0144] The hole stone dry granular glaze obtained in Examples 1-6 and Comparative Examples 1-3 is used as a sample, the sample is tested for the bending strength according to GB / T 4100-2015, and the test results are shown in Table 1.

[0145]

[0146] As shown in Table 1, the hole stone dry granular glaze prepared by the present application has good bending strength, can effectively resist external impact force, and thus effectively prolongs the service life of the glaze layer.

[0147] The above is only a preferred embodiment of the present application, and does not limit the present application in any form. Although the present application has been disclosed as above with a preferred embodiment, it is not intended to limit the present application. Any person skilled in the art can make some changes or modifications to the above disclosed technical content without departing from the scope of the technical solution of the present application, and any indirect modification, equivalent change and modification of the above embodiments according to the technical essence of the present application are still within the scope of the technical solution of the present application.

Claims

1. A dry granular glaze for hole stones, characterized by: The raw materials of the hole stone dry granular glaze include, by percentage, 58-62wt% solid raw materials, 0.3-0.5wt% hydroxyethyl cellulose, 0.16-0.2wt% sodium tripolyphosphate and the balance of water; The raw materials of the solid raw materials include, by percentage, 30-37wt% quartz sand, 18-26wt% potassium feldspar, 15-18wt% kaolin, 5-10wt% alumina-silicon microspheres coated with talc on the surface, 3-7wt% calcium oxide, 2-4wt% potassium oxide and the balance of zinc oxide; The preparation method of the alumina-silicon microspheres coated with talc on the surface comprises the following steps: Y1, uniformly mix talcum powder, silica sol and sodium hexametaphosphate to obtain talcum slurry; Y2, spray dry the silica sol, and calcine to obtain silica microspheres; Y3, after ultrasonic mixing of the silica microspheres and isopropyl alcohol, add aluminum sol dropwise, stir, centrifugal wash, and calcine to obtain alumina-silicon microspheres; Y4, mix the alumina-silicon microspheres, 3-aminopropyl triethoxysilane and ethanol solution to obtain alumina-silicon microspheres after coupling treatment; Y5, uniformly spray the talcum slurry on the alumina-silicon microspheres after coupling treatment, and calcine to obtain alumina-silicon microspheres coated with talc on the surface.

2. A dry granular glaze for a hole stone according to claim 1, wherein: The solid raw materials are 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 a speed of 200-300rpm for 3-5h, and then pass through a 40-60 mesh sieve to obtain premix; X2, uniformly mix the premix and alumina-silicon microspheres coated with talc on the surface to obtain solid raw materials.

3. A dry granular glaze for a hole stone according to claim 1, wherein: The talcum powder in step Y1 is obtained by ball milling talc at a speed of 250-350rpm for 1.5-2.5h, and then passing through a 60-80 mesh sieve; the mass ratio of the talcum powder, silica sol and sodium hexametaphosphate is 1:0.1-0.14:0.01-0.

03.

4. A dry granular glaze for a hole stone according to claim 1, wherein: The calcination in step Y2 refers to calcining at 950-1050℃ for 1.5-2.5h in an argon environment.

5. A dry granular glaze for a hole stone according to claim 1, wherein: The mass ratio of the microspheres, isopropyl alcohol 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 power to 200-400W, and ultrasonic mixing for 25-35min; the stirring refers to stirring at a speed of 300-400rpm for 1.5-2.5h at 58-62℃; and the calcination in step Y3 refers to calcining at 485-515℃ for 1-2h.

6. A dry granular glaze for a hole stone according to claim 1, wherein: The mass ratio of the alumina-silicon microspheres, 3-aminopropyl triethoxysilane and ethanol solution in step Y4 is 1:0.04-0.06:10-11; the ethanol solution is 88-92wt% ethanol solution; and the mixing in step Y4 refers to adjusting the pH to 5-6 and stirring at 60℃ for 2-3h.

7. A dry granular glaze for a hole stone according to claim 1, wherein: The mass ratio of the alumina-silicon microspheres after coupling treatment and talcum slurry in step Y5 is 1:1.1-1.3; and the calcination in step Y5 refers to calcining at 585-615℃ for 1-1.2h.

8. A method of preparing a hole stone dry granular glaze as claimed in any one of claims 1 to 7, characterized in that: The preparation method of the hole stone dry granular glaze comprises the following steps: Z1, after mixing the solid raw material, hydroxyethyl cellulose, sodium tripolyphosphate and water, stirring at 450-550 rpm for 1-2 h, dry granular glaze slurry is obtained; Z2, using the glaze spraying process, the dry granular glaze slurry is sprayed on the surface of the brick body at a specific gravity of 1.1-1.3 g / ml, 300 mm x 600 mm / plate, 30-40 g, and then calcined at 1140-1200 ℃ for 30-40 min.

Citation Information

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