Mirror-polished thin ceramic rock plate and preparation method thereof

Abstract

This invention discloses a mirror-polished thin ceramic slab and its preparation method, relating to the field of ceramics. In preparing the mirror-polished thin ceramic slab, this invention involves reacting octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane, and vinylpentamethyldisiloxane to obtain a polysiloxane; reacting 2-hydroxyethyl acrylate with cyanuric chloride to obtain a crosslinking agent; reacting the polysiloxane, crosslinking agent, chloropropane, and iodomethane to obtain a hydrophobic antibacterial coating material; and mixing the hydrophobic antibacterial coating material with a photoinitiator before coating it onto the surface of the ceramic slab and curing it under ultraviolet light. The mirror-polished thin ceramic slab prepared by this invention exhibits excellent antibacterial and hydrophobic properties.

Description

Technical Field

[0001] This invention relates to the field of ceramics, specifically to a mirror-polished thin ceramic slab and its preparation method. Background Technology

[0002] Ceramic slabs, originating in Europe, are a new type of building decoration material widely used in cabinets, furniture, floors, walls, and building facades due to their advantages such as wear resistance, acid and alkali corrosion resistance, fire resistance, high temperature resistance, aging resistance, slip resistance, water resistance, and diverse decorative options. However, ordinary ceramic slabs have poor oil resistance; some colored liquids can easily seep in, leaving obvious stains and affecting the aesthetics.

[0003] The mirror-polished thin ceramic slab prepared by this invention has good hydrophobic properties, can effectively reduce the adhesion of colored liquids, and has good antibacterial properties, thus having broad market prospects. Summary of the Invention

[0004] The purpose of this invention is to provide a method for preparing mirror-polished thin ceramic slabs to solve the problems existing in the prior art.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution:

[0006] A mirror-polished thin ceramic slab is prepared by mixing a hydrophobic antibacterial coating material and a photoinitiator 1173, coating the mixture onto the surface of the ceramic slab, and then curing it under ultraviolet light.

[0007] Preferably, the preparation method of the hydrophobic antibacterial coating material is as follows:

[0008] (1) Mix octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane and tetramethylammonium hydroxide siloxane, purge with nitrogen, stir at 200-300 r / min for 2-3 h at 80-90 °C, add vinylpentamethyldisiloxane at 0.2-0.4 times the mass of octamethylcyclotetrasiloxane, heat to 95-105 °C and stir for 7-9 h, then heat to 130-140 °C and stir for 40-60 min, vacuum distill for 1-2 h to obtain polysiloxane;

[0009] (2) Mix 2-hydroxyethyl acrylate, triethylamine and diethyl ether to prepare a mixed solution, and place it in a flask with a calcium chloride drying tube; add 3 to 4 times the mass of the mixed solution of cyanuric chloride solution to the flask with a calcium chloride drying tube, react at 0℃ for 10 to 14 h, filter, and extract the filtrate 2 to 4 times with 1 mol / L hydrochloric acid solution, 10% sodium bicarbonate solution and saturated sodium chloride solution respectively, and dry with sodium sulfate to obtain the crosslinking agent;

[0010] (3) Mix polysiloxane, chloropropane, iodomethane, crosslinking agent and toluene, and react at 75~85℃ to obtain coating material.

[0011] Preferably, the mass ratio of octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane and tetramethylammonium hydroxide siloxide in step (1) is 1:(0.4~0.6):(0.01~0.03).

[0012] Preferably, the mass ratio of 2-hydroxyethyl acrylate, triethylamine, and diethyl ether in step (2) is 1:(1~1.2):(1.5~2.5).

[0013] Preferably, the preparation method of the cyanuric chloride solution in step (2) is as follows: cyanuric chloride and diethyl ether are mixed at a mass ratio of 1:(1~2) to obtain the solution.

[0014] Preferably, the mass ratio of polysiloxane, chloropropane, iodomethane, crosslinking agent and toluene in step (2) is 1: (0.1~0.2): (0.01~0.02): (0.3~0.4): (10~20).

[0015] Preferably, the method for preparing the ceramic slab is as follows:

[0016] (1) Mix the raw materials of ceramic slab slurry, add water and pebbles, and then ball mill and sieve to obtain ceramic slab slurry.

[0017] (2) The ceramic slab slurry is spray-dried and aged to obtain ceramic slab powder;

[0018] (3) Press the ceramic slab blank powder into shape and dry it to obtain the ceramic slab blank;

[0019] (4) The ceramic slab blank is fired at high temperature, with a firing temperature of 1150~1250℃, a firing cycle of 50~150min, and a holding time of ≥7min at the highest firing temperature to obtain the ceramic slab.

[0020] Preferably, the raw material composition of the ceramic slab blank slurry is as follows: the chemical composition by weight percentage includes: SiO2 55%~65%, Al2O3 22%~28%, Fe2O3 0.6%~3%, CaO 0.5%~5.5%, MgO 0.5%~5%, K2O 1.5%~5%, Na2O 0.3%~2.3%, with the balance being impurities.

[0021] Compared with the prior art, the beneficial effects achieved by the present invention are:

[0022] In preparing mirror-polished thin ceramic slabs, this invention involves reacting octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane, and vinylpentamethyldisiloxane to obtain polysiloxane; reacting 2-hydroxyethyl acrylate with cyanuric chloride to obtain a crosslinking agent; reacting the polysiloxane, crosslinking agent, chloropropane, and iodomethane to obtain a hydrophobic antibacterial coating material; and mixing the hydrophobic antibacterial coating material with a photoinitiator before coating it onto the surface of the ceramic slab and curing it under ultraviolet light to obtain a mirror-polished thin ceramic slab.

[0023] First, polysiloxane is prepared by reacting octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane, and vinylpentamethyldisiloxane. The tertiary amine structure on 3-dimethylaminopropyl(dimethoxy)methylsilane can react with chloropropane to generate quaternary ammonium. Quaternary ammonium, as a cationic antibacterial monomer, can play a good antibacterial role and improve the antibacterial performance of mirror-polished thin ceramic slabs. Second, the polymethyl structure on polysiloxane can reduce surface energy, thereby effectively improving the hydrophobic properties of mirror-polished thin ceramic slabs. Detailed Implementation

[0024] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0025] Example 1:

[0026] A method for preparing a mirror-polished thin ceramic slab includes the following preparation steps:

[0027] 1. Preparation of hydrophobic antibacterial coating materials:

[0028] (1) Octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane and tetramethylammonium hydroxide siloxane were mixed in a mass ratio of 1:0.4:0.01, nitrogen gas was introduced, and the mixture was stirred at 200 r / min at 80°C for 2 h. Vinylpentamethyldisiloxane was added at a mass ratio of 0.2 times that of octamethylcyclotetrasiloxane, the temperature was raised to 95°C and stirred for 7 h, then the temperature was raised to 130°C and stirred for 40 min. The mixture was then vacuum distilled for 1 h to obtain polysiloxane.

[0029] (2) Mix 2-hydroxyethyl acrylate, triethylamine and diethyl ether in a mass ratio of 1:1:1.5 to prepare a mixed solution, and place it in a flask with a calcium chloride drying tube; mix cyanuric chloride and diethyl ether in a mass ratio of 1:1 to prepare a cyanuric chloride solution; add 3 times the mass of the mixed solution of cyanuric chloride solution to a flask with a calcium chloride drying tube, react at 0℃ for 10h, filter, and extract the filtrate twice with 1mol / L hydrochloric acid solution, 10% sodium bicarbonate solution and saturated sodium chloride solution respectively, and dry with sodium sulfate to obtain a crosslinking agent.

[0030] (3) Mix polysiloxane, chloropropane, iodomethane, crosslinking agent and toluene in a mass ratio of 1:0.1:0.01:0.3:10 and react at 75°C to obtain the coating material.

[0031] 2. Preparation method of ceramic slabs:

[0032] (1) Using SiO2 55%, Al2O3 22%, Fe2O3 0.6%, CaO 0.5%, MgO 0.5%, K2O 1.5% and Na2O 0.3% by mass as raw materials for ceramic slab body slurry, the raw materials for ceramic slab body slurry are mixed, and then water and pebbles are added. The mixture is then ball-milled through a ball milling system and sieved to obtain ceramic slab body slurry.

[0033] (2) The ceramic slab slurry is spray-dried and aged to obtain ceramic slab powder.

[0034] (3) Press the ceramic slab blank powder into shape and dry it to obtain the ceramic slab blank.

[0035] (4) The ceramic slab blank is fired at high temperature, with a firing temperature of 1150℃, a firing cycle of 500min, and a holding time of 9min at the highest firing temperature to obtain the ceramic slab.

[0036] 3. After mixing the hydrophobic antibacterial coating material and photoinitiator 1173, the mixture is applied to the surface of the ceramic slab and cured under ultraviolet light to obtain a mirror-polished thin ceramic slab.

[0037] Example 2:

[0038] A method for preparing a mirror-polished thin ceramic slab includes the following preparation steps:

[0039] 1. Preparation of hydrophobic antibacterial coating materials:

[0040] (1) Octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane and tetramethylammonium hydroxide siloxane were mixed at a mass ratio of 1:0.5:0.02, nitrogen gas was introduced, and the mixture was stirred at 250 r / min at 85°C for 2.5 h. Vinylpentamethyldisiloxane was added at a mass ratio of 0.3 times that of octamethylcyclotetrasiloxane, the temperature was raised to 100°C and stirred for 8 h, then the temperature was raised to 135°C and stirred for 50 min. The mixture was then vacuum distilled for 1.5 h to obtain polysiloxane.

[0041] (2) A mixed solution was prepared by mixing 2-hydroxyethyl acrylate, triethylamine and diethyl ether in a mass ratio of 1:1.1:2 and placed in a flask with a calcium chloride drying tube; a cyanuric chloride solution was prepared by mixing cyanuric chloride and diethyl ether in a mass ratio of 1:1.5; a cyanuric chloride solution with a mass of 3.5 times the mass of the mixed solution was added to a flask with a calcium chloride drying tube and reacted at 0℃ for 12 h. After filtration, the filtrate was extracted three times with 1 mol / L hydrochloric acid solution, 10% sodium bicarbonate solution and saturated sodium chloride solution respectively, and dried with sodium sulfate to obtain a crosslinking agent.

[0042] (3) Mix polysiloxane, chloropropane, iodomethane, crosslinking agent and toluene in a mass ratio of 1:0.15:0.015:0.35:15 and react at 80°C to obtain the coating material.

[0043] 2. Preparation method of ceramic slabs:

[0044] (1) Using SiO2 60%, Al2O3 25%, Fe2O3 1.8%, CaO 3%, MgO 2.75%, K2O 3.25% and Na2O 1.3% by mass as raw materials for ceramic slab body slurry, the raw materials for ceramic slab body slurry are mixed, and then water and pebbles are added. The mixture is then ball-milled through a ball milling system and sieved to obtain ceramic slab body slurry.

[0045] (2) The ceramic slab slurry is spray-dried and aged to obtain ceramic slab powder.

[0046] (3) Press the ceramic slab blank powder into shape and dry it to obtain the ceramic slab blank.

[0047] (4) The ceramic slab blank is fired at high temperature, with a firing temperature of 1200℃, a firing cycle of 100min, and a holding time of 9min at the highest firing temperature to obtain the ceramic slab.

[0048] 3. After mixing the hydrophobic antibacterial coating material and photoinitiator 1173, the mixture is applied to the surface of the ceramic slab and cured under ultraviolet light to obtain a mirror-polished thin ceramic slab.

[0049] Example 3:

[0050] A method for preparing a mirror-polished thin ceramic slab includes the following preparation steps:

[0051] 1. Preparation of hydrophobic antibacterial coating materials:

[0052] (1) Octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane and tetramethylammonium hydroxide siloxane were mixed in a mass ratio of 1:0.6:0.03, nitrogen gas was introduced, and the mixture was stirred at 300 r / min at 90°C for 3 h. Vinylpentamethyldisiloxane was added in 0.4 times the mass of octamethylcyclotetrasiloxane, the temperature was raised to 105°C and stirred for 9 h, then the temperature was raised to 140°C and stirred for 60 min. The mixture was then vacuum distilled for 2 h to obtain polysiloxane.

[0053] (2) A mixed solution was prepared by mixing 2-hydroxyethyl acrylate, triethylamine and diethyl ether in a mass ratio of 1:1.2:2.5 and placed in a flask with a calcium chloride drying tube; a cyanuric chloride solution was prepared by mixing cyanuric chloride and diethyl ether in a mass ratio of 1:2; a cyanuric chloride solution with a mass of 4 times the mass of the mixed solution was added to a flask with a calcium chloride drying tube and reacted at 0℃ for 14 h. After filtration, the filtrate was extracted 4 times with 1 mol / L hydrochloric acid solution, 10% sodium bicarbonate solution and saturated sodium chloride solution respectively, and dried with sodium sulfate to obtain the crosslinking agent.

[0054] (3) Mix polysiloxane, chloropropane, iodomethane, crosslinking agent and toluene in a mass ratio of 1:0.2:0.02:0.4:20 and react at 85°C to obtain the coating material.

[0055] 2. Preparation method of ceramic slabs:

[0056] (1) Using SiO2 65%, Al2O3 28%, Fe2O3 3%, CaO 5.5%, MgO 5%, K2O 5%, and Na2O 2.3% by mass as raw materials for ceramic slab body slurry, the raw materials for ceramic slab body slurry are mixed, and then water and pebbles are added. The mixture is then ball-milled through a ball milling system and sieved to obtain ceramic slab body slurry.

[0057] (2) The ceramic slab slurry is spray-dried and aged to obtain ceramic slab powder.

[0058] (3) Press the ceramic slab blank powder into shape and dry it to obtain the ceramic slab blank.

[0059] (4) The ceramic slab blank is fired at high temperature, with a firing temperature of 1250℃, a firing cycle of 150min, and a holding time of 9min at the highest firing temperature to obtain the ceramic slab.

[0060] 3. After mixing the hydrophobic antibacterial coating material and photoinitiator 1173, the mixture is applied to the surface of the ceramic slab and cured under ultraviolet light to obtain a mirror-polished thin ceramic slab.

[0061] Comparative Example 1:

[0062] A method for preparing a mirror-polished thin ceramic slab includes the following preparation steps:

[0063] 1. Preparation of hydrophobic antibacterial coating materials:

[0064] (1) Mix octamethylcyclotetrasiloxane and tetramethylammonium hydroxide siloxane at a mass ratio of 1:0.02, purge with nitrogen, stir at 250 r / min for 2.5 h at 85 °C, add vinylpentamethyldisiloxane at 0.3 times the mass of octamethylcyclotetrasiloxane, heat to 100 °C and stir for 8 h, then heat to 135 °C and stir for 50 min, vacuum distill for 1.5 h to obtain polysiloxane.

[0065] (2) A mixed solution was prepared by mixing 2-hydroxyethyl acrylate, triethylamine and diethyl ether in a mass ratio of 1:1.1:2 and placed in a flask with a calcium chloride drying tube; a cyanuric chloride solution was prepared by mixing cyanuric chloride and diethyl ether in a mass ratio of 1:1.5; a cyanuric chloride solution with a mass of 3.5 times the mass of the mixed solution was added to a flask with a calcium chloride drying tube and reacted at 0℃ for 12 h. After filtration, the filtrate was extracted three times with 1 mol / L hydrochloric acid solution, 10% sodium bicarbonate solution and saturated sodium chloride solution respectively, and dried with sodium sulfate to obtain a crosslinking agent.

[0066] (3) Mix polysiloxane, chloropropane, iodomethane, crosslinking agent and toluene in a mass ratio of 1:0.15:0.015:0.35:15 and react at 80°C to obtain the coating material.

[0067] 2. Preparation method of ceramic slabs:

[0068] (1) Using SiO2 60%, Al2O3 25%, Fe2O3 1.8%, CaO 3%, MgO 2.75%, K2O 3.25% and Na2O 1.3% by mass as raw materials for ceramic slab body slurry, the raw materials for ceramic slab body slurry are mixed, and then water and pebbles are added. The mixture is then ball-milled through a ball milling system and sieved to obtain ceramic slab body slurry.

[0069] (2) The ceramic slab slurry is spray-dried and aged to obtain ceramic slab powder.

[0070] (3) Press the ceramic slab blank powder into shape and dry it to obtain the ceramic slab blank.

[0071] (4) The ceramic slab blank is fired at high temperature, with a firing temperature of 1200℃, a firing cycle of 100min, and a holding time of 9min at the highest firing temperature to obtain the ceramic slab.

[0072] 3. After mixing the hydrophobic antibacterial coating material and photoinitiator 1173, the mixture is applied to the surface of the ceramic slab and cured under ultraviolet light to obtain a mirror-polished thin ceramic slab.

[0073] Comparative Example 2:

[0074] A method for preparing a ceramic slab includes the following preparation steps:

[0075] (1) Using SiO2 60%, Al2O3 25%, Fe2O3 1.8%, CaO 3%, MgO 2.75%, K2O 3.25% and Na2O 1.3% by mass as raw materials for ceramic slab body slurry, the raw materials for ceramic slab body slurry are mixed, and then water and pebbles are added. The mixture is then ball-milled through a ball milling system and sieved to obtain ceramic slab body slurry.

[0076] (2) The ceramic slab slurry is spray-dried and aged to obtain ceramic slab powder.

[0077] (3) Press the ceramic slab blank powder into shape and dry it to obtain the ceramic slab blank.

[0078] (4) The ceramic slab blank is fired at high temperature, with a firing temperature of 1200℃, a firing cycle of 100min, and a holding time of 9min at the highest firing temperature to obtain the ceramic slab.

[0079] Test Example 1:

[0080] Hydrophobicity test: The static contact angle of the prepared mirror-polished thin ceramic slab was tested using a static contact angle tester. The results are shown in Table 1.

[0081] Table 1. Statistics of hydrophobicity test results

[0082]

[0083] A comparison of the experimental data from Examples 1-3 and Comparative Examples 1 and 2 in Table 1 reveals that the mirror-polished thin ceramic slab prepared by this invention has good hydrophobic properties.

[0084] By comparison, the static contact angles of Examples 1-3 are greater than those of Comparative Example 2, indicating that the polysiloxane prepared by reacting octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane, and vinylpentamethyldisiloxane can reduce the surface energy, thereby effectively improving the hydrophobic properties of mirror-polished thin ceramic slabs.

[0085] Test Example 2:

[0086] Antibacterial performance test: The antibacterial performance of the samples against Escherichia coli was tested according to the standard method of JC / T897—2014 "Antibacterial Properties of Antibacterial Ceramic Products". The results are shown in Table 2.

[0087] Table 2. Statistics of Antibacterial Performance Test Results

[0088]

[0089] A comparison of the experimental data from Examples 1-3 and Comparative Examples 1 and 2 in Table 2 reveals that the mirror-polished thin ceramic slab prepared by this invention has good antibacterial properties.

[0090] By comparison, the antibacterial rates of Examples 1-3 were greater than those of Comparative Examples 1 and 2, indicating that polysiloxane was prepared by reacting octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane, and vinylpentamethyldisiloxane. The tertiary amine structure on 3-dimethylaminopropyl(dimethoxy)methylsilane can react with chloropropane to generate quaternary ammonium. Quaternary ammonium, as a cationic antibacterial monomer, can play a good antibacterial role and improve the antibacterial performance of mirror-polished thin ceramic slabs.

[0091] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of the present invention. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the scope of protection of the present invention. Any 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 mirror-polished thin ceramic rock plate, characterized in that, The mirror-polished thin ceramic slab is prepared by mixing a hydrophobic antibacterial coating material and photoinitiator 1173, coating the surface of the ceramic slab with ultraviolet light, and then curing it. The preparation method of the hydrophobic antibacterial coating material is as follows: (1) Mix octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane and tetramethylammonium hydroxide siloxane, purge with nitrogen, stir at 200-300 r / min for 2-3 h at 80-90 °C, add vinylpentamethyldisiloxane at 0.2-0.4 times the mass of octamethylcyclotetrasiloxane, heat to 95-105 °C and stir for 7-9 h, then heat to 130-140 °C and stir for 40-60 min, vacuum distill for 1-2 h to obtain polysiloxane; (2) Mix 2-hydroxyethyl acrylate, triethylamine and diethyl ether to prepare a mixed solution, and place it in a flask with a calcium chloride drying tube; add 3 to 4 times the mass of the mixed solution of cyanuric chloride solution to the flask with a calcium chloride drying tube, react at 0℃ for 10 to 14 h, filter, and extract the filtrate 2 to 4 times with 1 mol / L hydrochloric acid solution, 10% sodium bicarbonate solution and saturated sodium chloride solution respectively, and dry with sodium sulfate to obtain the crosslinking agent; (3) Mix polysiloxane, chloropropane, iodomethane, crosslinking agent and toluene, and react at 75~85℃ to obtain coating material; The mass ratio of octamethylcyclotetrasiloxane, 3-dimethylaminopropyl(dimethoxy)methylsilane and tetramethylammonium hydroxide silanolate in step (1) is 1:(0.4~0.6):(0.01~0.03). The mass ratio of 2-hydroxyethyl acrylate, triethylamine, and diethyl ether in step (2) is 1:(1~1.2):(1.5~2.5). The method for preparing the cyanuric chloride solution in step (2) is as follows: cyanuric chloride and diethyl ether are mixed at a mass ratio of 1:(1~2) to obtain the solution. The mass ratio of polysiloxane, chloropropane, iodomethane, crosslinking agent and toluene in step (3) is 1: (0.1~0.2): (0.01~0.02): (0.3~0.4): (10~20).

2. The mirror-polished thin ceramic stone plate according to claim 1, characterized in that, The method for preparing the ceramic slab is as follows: (1) Mix the raw materials of ceramic slab slurry, add water and pebbles, and then ball mill and sieve to obtain ceramic slab slurry. (2) The ceramic slab slurry is spray-dried and aged to obtain ceramic slab powder; (3) Press the ceramic slab blank powder into shape and dry it to obtain the ceramic slab blank; (4) The ceramic slab blank is fired at high temperature, with a firing temperature of 1150~1250℃, a firing cycle of 50~150min, and a holding time of ≥7min at the highest firing temperature to obtain the ceramic slab.

3. The mirror-polished thin ceramic stone plate according to claim 2, characterized in that, The raw material composition of the ceramic slab blank slurry is as follows: the chemical composition by weight percentage includes: SiO2 55%~65%, Al2O3 22%~28%, Fe2O3 0.6%~3%, CaO 0.5%~5.5%, MgO 0.5%~5%, K2O 1.5%~5%, Na2O 0.3%~2.3%, with the balance being impurities.

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