CN111892382A - Antibacterial and antiviral ceramic tile and preparation method thereof - Google Patents
Antibacterial and antiviral ceramic tile and preparation method thereof Download PDFInfo
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- CN111892382A CN111892382A CN202010796308.7A CN202010796308A CN111892382A CN 111892382 A CN111892382 A CN 111892382A CN 202010796308 A CN202010796308 A CN 202010796308A CN 111892382 A CN111892382 A CN 111892382A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N55/00—Biocides, pest repellants or attractants, or plant growth regulators, containing organic compounds containing elements other than carbon, hydrogen, halogen, oxygen, nitrogen and sulfur
- A01N55/02—Biocides, pest repellants or attractants, or plant growth regulators, containing organic compounds containing elements other than carbon, hydrogen, halogen, oxygen, nitrogen and sulfur containing metal atoms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/007—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by irradiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0056—Preparation of gels containing inorganic material and water
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0069—Post treatment
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20707—Titanium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/80—Type of catalytic reaction
- B01D2255/802—Photocatalytic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/06—Polluted air
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3436—Alkaline earth metal silicates, e.g. barium silicate
- C04B2235/3454—Calcium silicates, e.g. wollastonite
Abstract
The invention provides an antibacterial and antiviral ceramic tile and a preparation method thereof, wherein the ceramic tile comprises a blank body, a ground coat and a surface glaze, wherein the surface glaze comprises antibacterial and antiviral sol, and the raw materials of the antibacterial and antiviral sol comprise, by weight, 7-15 parts of tetrabutyl titanate, 0.2-0.4 part of an organic modifier, 0.3-0.6 part of a metal trace element complex and 0.2-0.4 part of an inorganic antibacterial agent. The ceramic tile has excellent antibacterial and antiviral effects, can absorb harmful gases in the air and purify the air, and is simple in preparation method and easy for industrial production.
Description
Technical Field
The invention belongs to the field of ceramic tiles, relates to a ceramic tile and a preparation method thereof, and particularly relates to an antibacterial and antiviral ceramic tile and a preparation method thereof.
Background
The ceramic tile is a practical decorative building material prepared by utilizing refractory metal oxides and semimetal oxides through a plurality of procedures of grinding, mixing, pressing, glazing, sintering and the like. Under the influence of new coronavirus pneumonia epidemic situation, people pay more attention to the health indexes of indoor decoration materials, and particularly common ceramic tiles are easy to adsorb viruses and breed bacteria, so that the health of human is seriously threatened. Moreover, the indoor air pollution is more and more serious at present, and particularly, most of various decoration materials contain formaldehyde which is a factor inducing many diseases at present. Therefore, the development of tiles capable of preventing epidemic, resisting bacteria and purifying air becomes the focus of research in the field of tiles.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides an antibacterial and antiviral ceramic tile and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention aims to provide an antibacterial and antiviral tile which comprises a blank body, a ground glaze and a surface glaze, wherein the surface glaze comprises antibacterial and antiviral sol, and the raw materials of the antibacterial and antiviral sol comprise, by weight, 7-15 parts of tetrabutyl titanate, 0.2-0.4 part of an organic modifier, 0.3-0.6 part of a metal trace element complex and 0.2-0.4 part of an inorganic antibacterial agent.
The amount of tetrabutyl titanate may be 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, etc., the amount of the organic modifier may be 0.22 part, 0.25 part, 0.28 part, 0.30 part, 0.32 part, 0.35 part, 0.38 part, etc., the amount of the metal trace element complex may be 0.35 part, 0.40 part, 0.45 part, 0.50 part, 0.55 part, etc., the amount of the inorganic antibacterial agent may be 0.22 part, 0.25 part, 0.28 part, 0.30 part, 0.32 part, 0.35 part, 0.38 part, etc., but is not limited to the above-mentioned values, and other values not listed in the above-mentioned values are also applicable.
In the invention, the metal trace element complex can cause the denaturation of virus nucleic acid and protein, inhibit the self-replication of virus and play the role of epidemic prevention; inorganic antibacterial agents have a broad spectrum of antibacterial properties and can provide a thorough and long-term antibacterial function. The tetrabutyl titanate can form nano titanium dioxide after being prepared, the nano titanium dioxide is an excellent photocatalyst material, and can effectively absorb and degrade toxic and harmful gases in the air such as formaldehyde and the like under the action of illumination so as to purify the indoor air.
As a preferable technical scheme of the invention, the blank comprises the following raw materials in parts by weight: 15-25 parts of clay, 5-8 parts of wollastonite, 0.5-1.2 parts of crushed pottery clay powder and 0.6-1.4 parts of diatomite.
The amount of clay may be 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 23 parts or 24 parts, the amount of wollastonite may be 5.5 parts, 6 parts, 6.5 parts, 7 parts or 7.5 parts, the amount of crushed clay may be 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1.0 parts or 1.1 parts, the amount of diatomaceous earth may be 0.7 parts, 0.8 parts, 0.9 parts, 1.0 parts, 1.1 parts, 1.2 parts or 1.3 parts, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned ranges are also applicable.
Preferably, the ground coat comprises the following raw materials in parts by weight: 14-18 parts of clay, 12-15 parts of feldspar, 14-18 parts of quartz and 5-7 parts of magnesium carbonate.
The clay may be 14.5 parts, 15 parts, 15.5 parts, 16 parts, 16.5 parts, 17 parts or 17.5 parts by weight, the feldspar may be 12.5 parts, 13 parts, 13.5 parts, 14 parts or 14.5 parts by weight, the quartz may be 14.5 parts, 15 parts, 15.5 parts, 16 parts, 16.5 parts, 17 parts or 17.5 parts by weight, the magnesium carbonate may be 5.2 parts, 5.5 parts, 5.8 parts, 6 parts, 6.2 parts, 6.5 parts or 6.8 parts by weight, but the present invention is not limited to the recited values, and other values not recited in the above ranges of values are also applicable.
Preferably, the overglaze comprises, by weight, 0.3-0.6 part of antibacterial and antiviral colloid, 15-20 parts of clay, 14-18 parts of feldspar, 5-8 parts of talc and 3-5 parts of quartz.
The antibacterial and antiviral colloid may be 0.35 parts, 0.40 parts, 0.45 parts, 0.50 parts or 0.55 parts by weight, the clay may be 16 parts, 17 parts, 18 parts or 19 parts by weight, the feldspar may be 15.5 parts, 16 parts, 16.5 parts, 17 parts or 17.5 parts by weight, the talc may be 5.5 parts, 6 parts, 6.5 parts, 7 parts or 7.5 parts by weight, the quartz may be 3.2 parts, 3.5 parts, 3.8 parts, 4 parts, 4.2 parts, 4.5 parts or 4.8 parts by weight, but is not limited to the recited values, and other values not recited in the above numerical ranges may be also applicable.
As a preferred embodiment of the present invention, the organic modifier comprises any one or a combination of at least two of polyvinylpyrrolidone, polyethylene glycol, urea or carboxymethylcellulose, and the combination is exemplified by, but not limited to: a combination of polyvinylpyrrolidone and polyethylene glycol, a combination of polyethylene glycol and urea, a combination of urea and carboxymethylcellulose, a combination of carboxymethylcellulose and polyvinylpyrrolidone, or a combination of polyvinylpyrrolidone, polyethylene glycol, urea and carboxymethylcellulose, and the like.
Preferably, the metal trace element complex comprises a phenanthroline complex of iron and/or a phenanthroline complex of rhodium.
Preferably, the inorganic antimicrobial agent comprises silver nitrate and/or zinc nitrate.
As a preferable technical scheme of the invention, the preparation method of the antibacterial and antiviral colloid comprises the following steps:
(1) mixing the tetrabutyl titanate with absolute ethyl alcohol, and adding an organic modifier for modification after mixing to obtain a solution A;
(2) mixing the metal trace element complex with absolute ethyl alcohol and water, and adjusting the pH to 3.5-4.5 by using an acid solution to obtain a solution B;
(3) mixing water and absolute ethyl alcohol, adjusting the pH to 3-4 by using an acid solution, and adding a sterile antibacterial agent to obtain a solution C;
(4) and dropwise adding the solution B and the solution C into the solution A, and aging to obtain the antibacterial and antiviral colloid.
In step (2), the pH may be 3.6, 3.7, 3.8, 3.9, 4.0, 4.1, 4.2, 4.3, or 4.4, etc., and in step (3), the pH may be 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, or 3.9, etc., but is not limited to the values recited, and other values not recited in the above ranges of values are also applicable.
In the present invention, the acid solution used for adjusting the pH may be any one of glacial acetic acid, dilute nitric acid, or dilute hydrochloric acid, or a combination of at least two thereof.
In a preferred embodiment of the present invention, the absolute ethyl alcohol in step (1) is 100 to 145 parts by weight, such as 105 parts, 110 parts, 115 parts, 120 parts, 125 parts, 130 parts, 135 parts, or 140 parts by weight, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the mixing in step (1) is performed under magnetic stirring, and the mixing time is 6-18 min, such as 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15min, 16min, or 17min, but not limited to the enumerated values, and other non-enumerated values in the range of the enumerated values are also applicable.
Preferably, the modification is performed under magnetic stirring after the organic modifier is added in step (1), and the modification time is 10-16 min, such as 11min, 12min, 13min, 14min or 15min, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
Preferably, the absolute ethyl alcohol in step (2) is 40 to 55 parts by weight, such as 42 parts, 45 parts, 48 parts, 50 parts, 52 parts or 54 parts by weight, and the water is 15 to 25 parts by weight, such as 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 23 parts or 24 parts by weight, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the mixing in step (2) is performed under magnetic stirring, and the mixing time is 35-45 min, such as 36min, 37min, 38min, 39min, 40min, 41min, 42min, 43min or 44min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the weight part of the absolute ethyl alcohol in the step (3) is 30 to 40 parts, and the weight part of the water is 1.5 to 3 parts, such as 1.6 parts, 1.8 parts, 2 parts, 2.2 parts, 2.5 parts or 2.8 parts, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the inorganic antibacterial agent in step (3) is added and then magnetically stirred for 6-12 min, such as 7min, 8min, 9min, 10min or 11min, but not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the dropping rate of the solution B in the step (4) is 65-80 drops/min, such as 66 drops/min, 68 drops/min, 70 drops/min, 72 drops/min, 75 drops/min or 78 drops/min, but not limited to the enumerated values, and other non-enumerated values in the numerical range are also applicable.
Preferably, the dropping rate of the solution C in the step (4) is 80-95 drops/min, such as 82 drops/min, 85 drops/min, 88 drops/min, 90 drops/min, 92 drops/min or 94 drops/min, but not limited to the enumerated values, and other non-enumerated values in the numerical range are also applicable.
Preferably, the dropping time in step (4) is 30-40 min, such as 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min or 39min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the aging time in step (4) is 25 to 30 hours, such as 25.5 hours, 26 hours, 26.5 hours, 27 hours, 27.5 hours, 28 hours, 28.5 hours, 29 hours or 29.5 hours, etc., but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In the invention, a sol-gel method is adopted to prepare uniform and stable gel capable of epidemic prevention, antibiosis and air purification; the gel is directly blended with the glaze material, thereby ensuring the complete combination of the glaze material and the film which can prevent epidemic, resist bacteria and purify air, and the gel is formed in one step, and is simple and convenient.
The invention also aims to provide a preparation method of the antibacterial and antiviral ceramic tile, which comprises the following steps:
(a) after ball milling, the raw material of the green body is mixed with water to prepare slurry, the slurry is pressed and molded in a mold, and the green body is obtained by sintering;
(b) ball-milling the raw materials of the ground glaze, adding water, mixing to prepare ground glaze, spraying the ground glaze on the surface of the blank in the step (a), and sintering to obtain a blank with the ground glaze;
(c) and ball-milling solid substances in the raw materials of the overglaze, adding water for mixing, adding the antibacterial and antiviral colloid in the mixing process to obtain the overglaze, spraying the overglaze on the blank with the ground glaze, and sintering to obtain the antibacterial and antiviral ceramic tile.
In a preferred embodiment of the present invention, the ball milling in step (a) is performed to 75 to 100 mesh, such as 80 mesh, 85 mesh, 90 mesh or 95 mesh, but the ball milling is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the sintering temperature in step (a) is 940-1180 ℃, such as 950 ℃, 980 ℃, 1000 ℃, 1020 ℃, 1050 ℃, 1080 ℃, 1100 ℃, 1120 ℃, 1150 ℃ or 1170 ℃, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
Preferably, the sintering time in step (a) is 36-48 h, such as 37h, 38h, 39h, 40h, 41h, 42h, 43h, 44h, 45h, 46h or 47h, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a preferred embodiment of the present invention, the ball milling time in step (b) is 12 to 14 hours, such as 12.2 hours, 12.5 hours, 12.8 hours, 13.0 hours, 13.2 hours, 13.5 hours, or 13.8 hours, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the sintering temperature in step (b) is 830-1100 ℃, such as 850 ℃, 880 ℃, 900 ℃, 920 ℃, 950 ℃, 980 ℃, 1000 ℃, 1020 ℃, 1050 ℃ or 1080 ℃, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the sintering time in step (b) is 24-30 h, such as 25h, 26h, 27h, 28h or 29h, but not limited to the recited values, and other values in the range are also applicable.
In a preferred embodiment of the present invention, the ball milling time in step (c) is 15 to 18 hours, such as 15.5 hours, 16 hours, 16.5 hours, 17 hours or 17.5 hours, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
Preferably, the sintering temperature in step (c) is 600-1190 ℃, such as 650 ℃, 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃ or 1150 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the sintering time in step (c) is 20-40 h, such as 22h, 25h, 28h, 30h, 32h, 35h or 38h, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferable technical scheme of the invention, the preparation method of the antibacterial and antiviral ceramic tile comprises the following steps:
(a) ball-milling raw materials of the blank to 75-100 meshes, adding water, mixing to prepare slurry, performing compression molding on the slurry in a mold, and sintering at 940-1180 ℃ for 36-48 hours to obtain the blank;
(b) ball-milling the raw materials of the ground glaze for 12-14 h, adding water, mixing to prepare ground glaze, spraying the ground glaze on the surface of the blank in the step (a), and sintering at 830-1100 ℃ for 24-30 h to obtain a blank with the ground glaze;
(c) and ball-milling solid substances in the raw materials of the overglaze for 15-18 h, adding water for mixing, adding the antibacterial and antiviral colloid in the mixing process to obtain overglaze, spraying the overglaze on the blank with the ground glaze, and sintering at 600-1190 ℃ for 20-40 h to obtain the antibacterial and antiviral ceramic tile.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the invention provides an antibacterial and antiviral ceramic tile which has excellent antibacterial and antiviral effects, wherein the killing rate of hepatitis B virus reaches over 99.3 percent, the killing rate of H5N1 avian influenza virus reaches about 99.7 percent, the bacteriostasis rate of staphylococcus aureus reaches over 99.6 percent, and the bacteriostasis rate of escherichia coli reaches over 99.6 percent;
(2) the invention provides an antibacterial and antiviral ceramic tile, which can effectively absorb and degrade toxic and harmful gases such as formaldehyde and the like in the air under the illumination effect, and purify the indoor air;
(3) the invention provides an antibacterial and antiviral ceramic tile, which is characterized in that a sol-gel method is adopted to prepare uniform and stable gel capable of epidemic prevention, antibiosis and air purification; the gel is directly blended with the glaze material, thereby ensuring the complete combination of the glaze material and the film which can prevent epidemic, resist bacteria and purify air, and the gel is formed in one step, and is simple and convenient.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of an antibacterial and antiviral ceramic tile, which comprises the following steps:
(a) ball-milling 16 parts by weight of clay, 5 parts by weight of wollastonite, 0.8 part by weight of broken clay powder and 1.1 part by weight of diatomite to 80-85 meshes, adding water, mixing to prepare slurry, carrying out compression molding on the slurry in a mold, and sintering at 1050 ℃ for 48 hours to obtain a blank;
(b) ball-milling 14 parts by weight of clay, 13 parts by weight of feldspar, 16 parts by weight of quartz and 6.5 parts by weight of magnesium carbonate for 12 hours, adding water, mixing to prepare a bottom glaze material, spraying the bottom glaze material on the surface of the blank in the step (a), and sintering at 900 ℃ for 24 hours to obtain a blank with the bottom glaze;
(c) and (2) ball-milling 17 parts by weight of clay, 17 parts by weight of feldspar, 5 parts by weight of talc and 3.5 parts by weight of quartz for 16 hours, adding water for mixing, adding 1 part by weight of the antibacterial and antiviral colloid in the mixing process to obtain a surface glaze material, and spraying the surface glaze material on the blank with the ground glaze and sintering at 830 ℃ for 23 hours to obtain the antibacterial and antiviral ceramic tile.
The preparation method of the antibacterial and antiviral colloid comprises the following steps:
(1) mixing 9 parts by weight of tetrabutyl titanate and 125 parts by weight of absolute ethyl alcohol under magnetic stirring for 10min, adding 0.35 part by weight of polyvinylpyrrolidone after mixing for modification, and carrying out magnetic stirring for 12min to obtain a solution A;
(2) mixing 0.3 part by weight of the phenanthroline complex of iron, 42 parts by weight of absolute ethyl alcohol and 16 parts by weight of deionized water, magnetically stirring for 40min, and adjusting the pH value to 4 by using an acid solution to obtain a solution B;
(3) mixing 2 parts by weight of water and 34 parts by weight of absolute ethyl alcohol, magnetically stirring for 8min, adjusting the pH to 3.5 by using an acid solution, adding 0.2 part by weight of silver nitrate, and magnetically stirring for 8min to obtain a solution C;
(4) and (3) dropwise adding the solution B and the solution C into the solution A at 72 drops/min and 88 drops/min respectively for 35min, and aging for 28h to obtain the antibacterial and antiviral colloid.
Example 2
The embodiment provides a preparation method of an antibacterial and antiviral ceramic tile, which comprises the following steps:
(a) ball-milling 15 parts by weight of clay, 7 parts by weight of wollastonite, 0.7 part by weight of broken clay powder and 1.1 part by weight of diatomite to 75-82 meshes, adding water, mixing to prepare slurry, carrying out compression molding on the slurry in a mold, and sintering at 980 ℃ for 42 hours to obtain a blank;
(b) ball milling 18 parts by weight of clay, 14 parts by weight of feldspar, 16 parts by weight of quartz and 6 parts by weight of magnesium carbonate for 14 hours, adding water, mixing to prepare a bottom glaze material, spraying the bottom glaze material on the surface of the blank in the step (a), and sintering at 1020 ℃ for 25 hours to obtain a blank with the bottom glaze;
(c) and (2) ball-milling 18 parts by weight of clay, 15 parts by weight of feldspar, 7 parts by weight of talc and 4 parts by weight of quartz for 15 hours, adding water for mixing, adding 1.5 parts by weight of the antibacterial and antiviral colloid in the mixing process to obtain a surface glaze material, and spraying the surface glaze material on the blank with the ground glaze and sintering at 960 ℃ for 32 hours to obtain the antibacterial and antiviral ceramic tile.
The preparation method of the antibacterial and antiviral colloid comprises the following steps:
(1) mixing 10 parts by weight of tetrabutyl titanate and 110 parts by weight of absolute ethyl alcohol under magnetic stirring for 8min, adding 0.3 part by weight of carboxymethyl cellulose after mixing for modification, and carrying out magnetic stirring for 10min to obtain a solution A;
(2) mixing 0.4 part by weight of the phenanthroline complex of rhodium, 44 parts by weight of absolute ethyl alcohol and 18 parts by weight of deionized water, magnetically stirring for 30min, and adjusting the pH value to 3.5 by using an acid solution to obtain a solution B;
(3) mixing 2.5 parts by weight of water and 40 parts by weight of absolute ethyl alcohol, magnetically stirring for 10min, adjusting the pH to 3.5 by using an acid solution, adding 0.3 part by weight of silver nitrate, and magnetically stirring for 12min to obtain a solution C;
(4) and (3) dropwise adding the solution B and the solution C into the solution A at 80 drops/min and 84 drops/min respectively for 40min, and aging for 30h to obtain the antibacterial and antiviral colloid.
Example 3
The embodiment provides a preparation method of an antibacterial and antiviral ceramic tile, which comprises the following steps:
(a) ball-milling 23 parts by weight of clay, 8 parts by weight of wollastonite, 1.3 parts by weight of broken clay powder and 1.0 part by weight of diatomite to 80-90 meshes, adding water, mixing to prepare slurry, carrying out compression molding on the slurry in a mold, and sintering at 1100 ℃ for 36 hours to obtain the blank;
(b) ball milling 15 parts by weight of clay, 12 parts by weight of feldspar, 15 parts by weight of quartz and 5 parts by weight of magnesium carbonate for 14 hours, adding water, mixing to prepare a bottom glaze material, spraying the bottom glaze material on the surface of the blank in the step (a), and sintering at 1050 ℃ for 25 hours to obtain a blank with the bottom glaze;
(c) 16.5 parts of clay, 15 parts of feldspar, 6.5 parts of talc and 4.5 parts of quartz are subjected to ball milling for 18 hours and then mixed with water, 1 part of antibacterial and antiviral colloid is added in the mixing process to obtain a surface glaze material, and the blank with the ground glaze is sprayed with the surface glaze material 1180 ℃ and sintered for 27 hours to obtain the antibacterial and antiviral ceramic tile.
The preparation method of the antibacterial and antiviral colloid comprises the following steps:
(1) mixing 8 parts by weight of tetrabutyl titanate and 105 parts by weight of absolute ethyl alcohol under magnetic stirring for 15min, adding 0.4 part by weight of urea after mixing for modification, and stirring for 15min under magnetic stirring to obtain a solution A;
(2) mixing 0.6 part by weight of phenanthroline complex of rhodium, 54 parts by weight of absolute ethyl alcohol and 22 parts by weight of deionized water, magnetically stirring for 42min, and adjusting the pH value to 4.5 by using an acid solution to obtain a solution B;
(3) mixing 2.5 parts by weight of water and 38 parts by weight of absolute ethyl alcohol, magnetically stirring for 12min, adjusting the pH to 3 by using an acid solution, adding 0.2 part by weight of zinc nitrate, and magnetically stirring for 10min to obtain a solution C;
(4) and (3) dropwise adding the solution B and the solution C into the solution A at 72 drops/min and 84 drops/min respectively for 32min, and aging for 28h to obtain the antibacterial and antiviral colloid.
Example 4
The embodiment provides a preparation method of an antibacterial and antiviral ceramic tile, which comprises the following steps:
(a) ball-milling 21 parts by weight of clay, 6.5 parts by weight of wollastonite, 1 part by weight of broken clay powder and 1.1 part by weight of diatomite to 75-80 meshes, adding water, mixing to prepare slurry, performing compression molding on the slurry in a mold, and sintering at 955 ℃ for 44 hours to obtain a blank;
(b) ball milling 18 parts by weight of clay, 13 parts by weight of feldspar, 14 parts by weight of quartz and 7 parts by weight of magnesium carbonate for 12 hours, adding water, mixing to prepare a bottom glaze material, spraying the bottom glaze material on the surface of the blank in the step (a), and sintering at 980 ℃ for 29 hours to obtain a blank with the bottom glaze;
(c) ball-milling 19 parts by weight of clay, 15 parts by weight of feldspar, 8 parts by weight of talc and 5 parts by weight of quartz for 17 hours, adding water for mixing, adding 2 parts by weight of the antibacterial and antiviral colloid in the mixing process to obtain a surface glaze material, and spraying the surface glaze material on the blank with the ground glaze and sintering at 1100 ℃ for 36 hours to obtain the antibacterial and antiviral ceramic tile.
The preparation method of the antibacterial and antiviral colloid comprises the following steps:
(1) mixing 13 parts by weight of tetrabutyl titanate and 145 parts by weight of absolute ethyl alcohol under magnetic stirring for 8min, adding 0.35 part by weight of polyethylene glycol after mixing for modification, and stirring for 12min under magnetic stirring to obtain a solution A;
(2) mixing 0.55 part by weight of the phenanthroline complex of iron, 52 parts by weight of absolute ethyl alcohol and 24 parts by weight of deionized water, magnetically stirring for 40min, and adjusting the pH to 3.5 by using an acid solution to obtain a solution B;
(3) mixing 2 parts by weight of water and 38 parts by weight of absolute ethyl alcohol, magnetically stirring for 10min, adjusting the pH to 4 by using an acid solution, adding 0.25 part by weight of silver nitrate, and magnetically stirring for 8min to obtain a solution C;
(4) and (3) dropwise adding the solution B and the solution C into the solution A at 65 drops/min and 85 drops/min respectively, wherein the dropwise adding time is 34min, and aging for 30h to obtain the antibacterial and antiviral colloid.
Comparative example
In this comparative example, the conditions were the same as in example 1 except that tetrabutyl titanate, an organic modifier, a metal trace element complex and an inorganic antibacterial agent were directly added to the overglaze instead of being added to the overglaze as a gel prepared by a sol-gel method.
The antibacterial and antiviral properties of the tiles provided in examples 1 to 4 and the comparative example were tested, and the results of the antiviral property test are shown in table 1 and the results of the antibacterial property test are shown in table 2.
The test method of the killing rate of the hepatitis B virus is DNA quantitative detection, and the source of the hepatitis B virus is a hepatitis B virus library.
The test method of the killing rate of the H5N1 avian influenza virus is an NASBA detection method, and the source of the H5N1 avian influenza virus is diseased local chickens.
Coli antibacterial rate was measured by plate counting method, and the source of e.coli was e.coli (ATCC 25922).
The test method for staphylococcus aureus was plate counting, and the source of staphylococcus aureus was s.
TABLE 1
| Example No. 2 | Killing rate of hepatitis B virus | Killing rate to H5N1 avian influenza virus |
| Example 1 | 99.34％ | 99.8％ |
| Example 2 | 99.46％ | 99.7％ |
| Example 3 | 99.42％ | 99.8％ |
| Example 4 | 99.55％ | 99.6％ |
| Comparative example | 0 | 0 |
TABLE 2
As can be seen from the test results in tables 1 and 2, the antibacterial and antiviral tiles provided in examples 1 to 4 of the present invention have excellent killing rates of more than 99% for hepatitis b virus and H5N1 avian influenza virus, and also have excellent antibacterial rates of more than 99% for escherichia coli and staphylococcus aureus. In the comparative example, tetrabutyl titanate, an organic modifier, a metal trace element complex and an inorganic antibacterial agent are directly added into the overglaze instead of being prepared into gel by a sol-gel method and added into the overglaze, so that the fusion of the materials and the overglaze is extremely poor, and the corresponding antibacterial and disease-resistant effects can hardly be exerted.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The antibacterial and antiviral ceramic tile is characterized by comprising a blank body, a ground glaze and a surface glaze, wherein the surface glaze comprises antibacterial and antiviral sol, and the raw materials of the antibacterial and antiviral sol comprise, by weight, 7-15 parts of tetrabutyl titanate, 0.2-0.4 part of an organic modifier, 0.3-0.6 part of a metal trace element complex and 0.2-0.4 part of an inorganic antibacterial agent.
2. The antibacterial and antiviral ceramic tile according to claim 1, wherein the blank comprises the following raw materials in parts by weight: 15-25 parts of clay, 5-8 parts of wollastonite, 0.5-1.2 parts of crushed pottery clay powder and 0.6-1.4 parts of diatomite;
preferably, the ground coat comprises the following raw materials in parts by weight: 14-18 parts of clay, 12-15 parts of feldspar, 14-18 parts of quartz and 5-7 parts of magnesium carbonate;
preferably, the overglaze comprises, by weight, 0.3-0.6 part of antibacterial and antiviral colloid, 15-20 parts of clay, 14-18 parts of feldspar, 5-8 parts of talc and 3-5 parts of quartz.
3. The antibacterial and antiviral tile according to claim 1 or 2, wherein the organic modifier comprises any one or a combination of at least two of polyvinylpyrrolidone, polyethylene glycol, urea or carboxymethyl cellulose;
preferably, the metal trace element complex comprises a phenanthroline complex of iron and/or a phenanthroline complex of rhodium;
preferably, the inorganic antimicrobial agent comprises silver nitrate and/or zinc nitrate.
4. The antibacterial and antiviral tile according to any one of claims 1 to 3, wherein the preparation method of the antibacterial and antiviral colloid comprises the following steps:
(1) mixing the tetrabutyl titanate with absolute ethyl alcohol, and adding an organic modifier for modification after mixing to obtain a solution A;
(2) mixing the metal trace element complex with absolute ethyl alcohol and water, and adjusting the pH to 3.5-4.5 by using an acid solution to obtain a solution B;
(3) mixing water and absolute ethyl alcohol, adjusting the pH to 3-4 by using an acid solution, and adding a sterile antibacterial agent to obtain a solution C;
(4) and dropwise adding the solution B and the solution C into the solution A, and aging to obtain the antibacterial and antiviral colloid.
5. The antibacterial and antiviral tile according to claim 4, wherein the weight parts of the absolute ethyl alcohol in the step (1) are 100-145 parts;
preferably, the mixing in the step (1) is carried out under magnetic stirring, and the mixing time is 6-18 min;
preferably, after the organic modifier is added in the step (1), modification is carried out under magnetic stirring, and the modification time is 10-16 min;
preferably, the weight part of the absolute ethyl alcohol in the step (2) is 40-55 parts, and the weight part of the water is 15-25 parts;
preferably, the mixing in the step (2) is carried out under magnetic stirring, and the mixing time is 35-45 min;
preferably, the weight part of the absolute ethyl alcohol in the step (3) is 30-40 parts, and the weight part of the water is 1.5-3 parts;
preferably, after the inorganic antibacterial agent in the step (3) is added, magnetic stirring is carried out for 6-12 min;
preferably, the dropping rate of the solution B in the step (4) is 65-80 drops/min;
preferably, the dropping rate of the solution C in the step (4) is 80-95 drops/min;
preferably, the dripping time in the step (4) is 30-40 min;
preferably, the aging treatment time in the step (4) is 25-30 h.
6. A method for preparing the antibacterial and antiviral tile according to any one of claims 1 to 5, wherein the method comprises the steps of:
(a) after ball milling, the raw material of the green body is mixed with water to prepare slurry, the slurry is pressed and molded in a mold, and the green body is obtained by sintering;
(b) ball-milling the raw materials of the ground glaze, adding water, mixing to prepare ground glaze, spraying the ground glaze on the surface of the blank in the step (a), and sintering to obtain a blank with the ground glaze;
(c) and ball-milling solid substances in the raw materials of the overglaze, adding water for mixing, adding the antibacterial and antiviral colloid in the mixing process to obtain the overglaze, spraying the overglaze on the blank with the ground glaze, and sintering to obtain the antibacterial and antiviral ceramic tile.
7. The preparation method according to claim 6, wherein the ball milling in the step (a) is carried out to 75-100 meshes;
preferably, the sintering temperature of the step (a) is 940-1180 ℃;
preferably, the sintering time in the step (a) is 36-48 h.
8. The preparation method of claim 6 or 7, wherein the ball milling time in the step (b) is 12-14 h;
preferably, the sintering temperature of the step (b) is 830-1100 ℃;
preferably, the sintering time in the step (b) is 24-30 h.
9. The preparation method according to any one of claims 6 to 8, wherein the time for ball milling in step (c) is 15 to 18 hours;
preferably, the sintering temperature of the step (c) is 600-1190 ℃;
preferably, the sintering time in the step (c) is 20-40 h.
10. The method for preparing according to any one of claims 6 to 9, characterized in that it comprises the steps of:
(a) ball-milling raw materials of the blank to 75-100 meshes, adding water, mixing to prepare slurry, performing compression molding on the slurry in a mold, and sintering at 940-1180 ℃ for 36-48 hours to obtain the blank;
(b) ball-milling the raw materials of the ground glaze for 12-14 h, adding water, mixing to prepare ground glaze, spraying the ground glaze on the surface of the blank in the step (a), and sintering at 830-1100 ℃ for 24-30 h to obtain a blank with the ground glaze;
(c) and ball-milling solid substances in the raw materials of the overglaze for 15-18 h, adding water for mixing, adding the antibacterial and antiviral colloid in the mixing process to obtain overglaze, spraying the overglaze on the blank with the ground glaze, and sintering at 600-1190 ℃ for 20-40 h to obtain the antibacterial and antiviral ceramic tile.
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