CN117024119A - Preparation method of self-cleaning glazed ceramic cup - Google Patents
Preparation method of self-cleaning glazed ceramic cup Download PDFInfo
- Publication number
- CN117024119A CN117024119A CN202311304456.2A CN202311304456A CN117024119A CN 117024119 A CN117024119 A CN 117024119A CN 202311304456 A CN202311304456 A CN 202311304456A CN 117024119 A CN117024119 A CN 117024119A
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- ceramic cup
- self
- cleaning
- glazed ceramic
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- 239000000919 ceramic Substances 0.000 title claims abstract description 94
- 238000004140 cleaning Methods 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 82
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- XEFQLINVKFYRCS-UHFFFAOYSA-N Triclosan Chemical compound OC1=CC(Cl)=CC=C1OC1=CC=C(Cl)C=C1Cl XEFQLINVKFYRCS-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000011248 coating agent Substances 0.000 claims abstract description 24
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
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- 229940089951 perfluorooctyl triethoxysilane Drugs 0.000 claims description 16
- AVYKQOAMZCAHRG-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AVYKQOAMZCAHRG-UHFFFAOYSA-N 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
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- 239000008096 xylene Substances 0.000 claims description 10
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims description 7
- 239000004113 Sepiolite Substances 0.000 claims description 7
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 7
- 229910033181 TiB2 Inorganic materials 0.000 claims description 7
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 7
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 7
- 229910052624 sepiolite Inorganic materials 0.000 claims description 7
- 235000019355 sepiolite Nutrition 0.000 claims description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 7
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- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims description 6
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000010881 fly ash Substances 0.000 claims description 6
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- 229910052851 sillimanite Inorganic materials 0.000 claims description 6
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- 239000010456 wollastonite Substances 0.000 claims description 6
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- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 claims description 5
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
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Classifications
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- C04B33/00—Clay-wares
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- C04B33/04—Clay; Kaolin
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- A—HUMAN NECESSITIES
- A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
- A47G—HOUSEHOLD OR TABLE EQUIPMENT
- A47G19/00—Table service
- A47G19/22—Drinking vessels or saucers used for table service
- A47G19/2205—Drinking glasses or vessels
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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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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- 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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- 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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- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3213—Strontium oxides or oxide-forming salts thereof
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- C04B2235/3436—Alkaline earth metal silicates, e.g. barium silicate
- C04B2235/3454—Calcium silicates, e.g. wollastonite
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- C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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- C04B2235/602—Making the green bodies or pre-forms by moulding
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6565—Cooling rate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Abstract
The invention belongs to the technical field of ceramic cup preparation, and particularly relates to a preparation method of a self-cleaning glazing ceramic cup. The preparation method of the self-cleaning glazed ceramic cup comprises the following steps: (1) preparing a ceramic cup blank; (2) preparing a glazed ceramic cup; (3) Preparing a mixture of modified nano zirconia and cellulose nano fibers; (4) Preparing a 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution; (5) preparing self-cleaning coating liquid; (6) And spraying the prepared self-cleaning coating liquid on the glazed ceramic cup, and then drying to prepare the self-cleaning glazed ceramic cup. The preparation method of the self-cleaning glazed ceramic cup has the advantages that the technological parameters are easy to control, industrial production can be realized, and the prepared ceramic cup has excellent wear resistance, self-cleaning property and antibacterial property.
Description
Technical Field
The invention belongs to the technical field of ceramic cup preparation, and particularly relates to a preparation method of a self-cleaning glazing ceramic cup.
Background
Ceramic glaze is a thin layer of colorless or colored glass state that covers the surface of the ceramic article. The ceramic glaze is prepared by mixing mineral raw materials and chemical raw materials according to a certain proportion, finely grinding to prepare glaze slurry, coating the glaze slurry on a ceramic blank, and calcining. The ceramic glaze has the main functions of antifouling and decoration, so that the texture of the ceramic surface is soft, elegant, bright and clean, and the ceramic is provided with culture, spirit and life by matching with the innovation of the design, and has more life feeling.
The self-cleaning ceramic material is a ceramic material which can realize spontaneous separation performance under the external natural environment (solar energy, rainwater, wind power and the like) by only depending on the physical or chemical properties of the ceramic surface without external strong scrubbing of pollutants, chemical agents such as detergents and the like.
The photocatalysis self-cleaning is the most common self-cleaning ceramic material at present, and the photocatalysis self-cleaning ceramic is a multifunctional environment-friendly ceramic which has the functions of stable sterilization, degradation of organic pollutants and keeping the surface of the ceramic clean, and is different from the common ceramic in that the surface of the photocatalysis self-cleaning ceramic is plated with a photocatalyst film of tens of nanometers or hundreds of nanometers. The photocatalyst film is typically made of doped TiO 2 The composition is activated under ultraviolet irradiation and has normal-temperature deep oxidation-reduction capability, thereby generating self-cleaning function. However, the binding force between the photocatalyst film and the glaze layer is poor, and the photocatalyst film can only play a role under the irradiation of ultraviolet light, and the use condition is severe, so that a novel preparation method of the self-cleaning glazed ceramic cup is necessary to be explored.
Disclosure of Invention
The purpose of the invention is that: provides a preparation method of a self-cleaning glazed ceramic cup. The ceramic cup prepared by the method has wear resistance, self-cleaning property and antibacterial property.
The preparation method of the self-cleaning glazed ceramic cup provided by the invention comprises the following steps:
(1) Uniformly mixing the raw materials of the green body, performing wet ball milling and drying to obtain powder, and performing compression molding on the powder to obtain a ceramic cup green body;
(2) Spreading slurry on the surface of a ceramic cup blank to form a glaze layer, drying and firing, and finally cooling to room temperature at a cooling rate of 10-12 ℃/h to prepare a glazed ceramic cup;
(3) Adding nano zirconia and cellulose nano fiber into a mixed solution composed of absolute ethyl alcohol and water, stirring for 45-50min at 50-55 ℃, then adding sodium hydroxide to adjust the pH value of a reaction system to 8, and continuing stirring for 1.5-1.7h; finally adding perfluorooctyl triethoxysilane, continuously stirring for 2.5-3 hours at 50-55 ℃, filtering the reaction product, and drying for 1.2-1.5 hours at 60-65 ℃ to prepare a mixture of modified nano zirconia and cellulose nano fibers;
(4) Dissolving 5-chloro-2- (2, 4-dichlorophenoxy) phenol in a xylene solution, and stirring for 15-20min at 62-65 ℃ to prepare a 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution;
(5) Adding polyvinylidene fluoride-hexafluoropropylene copolymer into polytetrafluoroethylene emulsion, stirring for 30-35min at 150-155 ℃, cooling to 62-65 ℃, adding the mixture of modified nano zirconia and cellulose nano fiber prepared in the step (3) and the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution prepared in the step (4), stirring and mixing for 40-45min, and preparing the self-cleaning coating liquid;
(6) Spraying the self-cleaning coating liquid prepared in the step (5) on the glazed ceramic cup prepared in the step (2), and then drying to prepare the self-cleaning glazed ceramic cup.
Wherein:
the ceramic cup blank in the step (1) is composed of the following raw materials in parts by weight: 28-30 parts of bentonite, 18-20 parts of cordierite, 15-17 parts of wollastonite, 9-11 parts of perlite, 3-5 parts of fly ash, 7-9 parts of potassium feldspar, 3-5 parts of strontium carbonate, 4-5 parts of silicon nitride and 6-7 parts of sepiolite.
Strontium carbonate, silicon nitride and sepiolite are additionally added into the ceramic cup blank, the addition of the strontium carbonate reduces the firing shrinkage rate of the blank, the wear resistance and toughness of the blank are enhanced, the addition of the silicon nitride enhances the corrosion resistance of the ceramic cup blank, and the addition of the sepiolite can improve the plasticity, the bonding performance and the drying strength of the blank pug; the raw materials are compounded and used for enhancing the compactness of the ceramic cup blank, so that the ceramic cup blank is ensured to have good structural compactness.
The mass of water added during wet ball milling in the step (1) accounts for 30 percent of the sum of the mass of the blank raw material and the mass of water, and the ball milling time is 20 hours.
The drying temperature in the step (1) is 105 ℃ and the drying time is 10 hours.
The pressure of the compression molding in the step (1) is 70MPa.
The glaze layer in the step (2) consists of the following raw materials in parts by weight: 10-12 parts of nepheline, 8-10 parts of talcum, 12-14 parts of sillimanite, 1-3 parts of calcite, 11-13 parts of celsian, 6-8 parts of coal gangue, 13-15 parts of pyrophyllite, 5-7 parts of titanium nitride, 7-8 parts of calcium carbide gas powder and 2-4 parts of titanium diboride.
The pyrophyllite, titanium nitride, tourmaline powder and titanium diboride are added in the glaze layer, so that the thermal expansion rate of the pyrophyllite is low, the firing temperature can be reduced, the rapid firing of the ceramic cup is promoted, and the prepared ceramic cup has small shrinkage and high strength; the addition of titanium nitride can improve the wear resistance of the glaze layer; the addition of tourmaline powder ensures that the glaze layer has certain easy cleaning property, and improves the whiteness and glossiness of the glaze surface; the addition of titanium diboride plays a role in grain refinement, and ensures the compactness and mechanical strength of the glaze layer.
The slurry in the step (2) is prepared by ball milling the glaze raw material by a wet method and sieving the glaze raw material by a 350-mesh sieve, wherein the mass of added water accounts for 50% of the sum of the mass of water and the glaze raw material.
The drying temperature in the step (2) is 113 ℃, and the drying time is 2.5h.
The firing in the step (2) is carried out by heating from room temperature to 550-560 ℃ for 50-60min at a heating rate of 8 ℃/min, then heating to 850-860 ℃ for 45-55min at a heating rate of 5 ℃/min, and finally heating to 1250-1255 ℃ for 2-2.2h at a heating rate of 3 ℃/min.
The volume ratio of the absolute ethyl alcohol to the water in the step (3) is 25:1; the volume ratio of perfluorooctyl triethoxysilane to water is 1:1.
In the step (3), the mass sum of the nano zirconia and the cellulose nano fiber and the volume ratio of the nano zirconia to the perfluorooctyl triethoxysilane are 35:8, and the unit is g/mL.
In the step (3), the mass ratio of the nano zirconia to the cellulose nano fiber is 1:0.7-0.8.
In the step (4), the mass ratio of the 5-chloro-2- (2, 4-dichlorophenoxy) phenol to the xylene solution is 1:1.
The mass ratio of the polyvinylidene fluoride-hexafluoropropylene copolymer to the polytetrafluoroethylene emulsion in the step (5) is 0.4-0.6:1.5-1.8.
The mass ratio of the mixture of the modified nano zirconia and the cellulose nano fiber to the polytetrafluoroethylene emulsion in the step (5) is 0.2-0.3:1.
In the step (5), the mass ratio of the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution to the polytetrafluoroethylene emulsion is 0.05-0.08:1.
In the step (6), the drying temperature is 110-115 ℃ and the drying time is 6-7h.
In the self-cleaning coating liquid, nano zirconia and cellulose nano fiber are compounded for use, and the self-cleaning coating liquid is endowed with hydrophobic property through modification treatment of perfluorooctyl triethoxysilane; wherein, the nano zirconia can generate conduction band electrons and valence band holes under the illumination condition, the holes have attraction effect on electrons, have oxidizing capability and strong reactivity, and can be adsorbed with H on the surface 2 O or OH ions react to form hydroxyl with strong oxidability, cells are killed by the strong oxidability of the hydroxyl, cell membranes can be penetrated, membrane structures are damaged, toxins produced by the cells are reduced, and therefore a sterilizing effect is achieved; the cellulose nanofiber has high length-diameter ratio, is easy to form a micro-network structure, and provides favorable conditions for forming a surface roughness structure of the super-hydrophobic coating. Because the nano zirconia has the premise of sterilization, the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution is additionally added, so that the prepared ceramic cup has the antibacterial and sterilization effects on the premise of no illumination, and has good inhibition effects on gram-positive bacteria, gram-negative bacteria, mold and the like. The mixed solution composed of polyvinylidene fluoride-hexafluoropropylene copolymer and polytetrafluoroethylene emulsion has good superhydrophobicity, wear resistance, oxidation resistance and weather resistance, the mixture of modified nano zirconia and cellulose nano fiber is added into the mixed solution, a micro network structure is formed on the surface of the superhydrophobic coating, and the surface of the mixture is roughened, so that the surface is further improvedSelf-cleaning capability. Because the prepared self-cleaning coating liquid has good superhydrophobicity and micro-coarse structure, pollutants can be easily removed under the action of external force under the superhydrophobicity.
Compared with the prior art, the invention has the following beneficial effects:
(1) The preparation method of the self-cleaning glazed ceramic cup has the advantages that the technological parameters are easy to control, the industrial production can be realized, and the prepared ceramic cup has excellent self-cleaning performance.
(2) The self-cleaning glazed ceramic cup prepared by the method disclosed by the invention has the advantages that the green body layer, the glaze layer and the self-cleaning coating are matched and cooperated, the green body layer ensures the compactness of the ceramic cup green body through the interaction between raw materials, so that the self-cleaning performance of the ceramic cup is assisted, the glaze layer has certain easy cleaning property and mechanical strength through the interaction between raw materials of the glaze layer, and the self-cleaning coating is matched with a micro-rough structure formed by the mixture of the modified nano zirconia and the cellulose nano fiber through the superhydrophobicity of the coating, so that the wear resistance, self-cleaning property and antibacterial property of the glazed ceramic cup are ensured.
Detailed Description
The invention is further described below with reference to examples.
The manufacturer of cellulose nano-fiber is northern century (Jiangsu) cellulose materials limited company; the manufacturer of the polyvinylidene fluoride-hexafluoropropylene copolymer is manufactured by the Acemax France, and the model is Kynar Flex 2850; the manufacturer of the polytetrafluoroethylene emulsion is Guangzhou pine and cypress chemical industry Co., ltd, and the solid content is 60%.
Example 1
The preparation method of the self-cleaning glazed ceramic cup of the embodiment 1 comprises the following steps:
(1) Uniformly mixing the raw materials of the green body, performing wet ball milling and drying to obtain powder, and performing compression molding on the powder to obtain a ceramic cup green body;
(2) Spreading slurry on the surface of a ceramic cup blank to form a glaze layer, drying and firing, and finally cooling to room temperature at a cooling rate of 11 ℃/h to prepare a glazed ceramic cup;
(3) Adding nano zirconia and cellulose nano fiber into a mixed solution composed of absolute ethyl alcohol and water, stirring for 47min at 53 ℃, then adding sodium hydroxide to adjust the pH value of a reaction system to 8, and continuing stirring for 1.6h; finally, adding perfluorooctyl triethoxysilane, continuously stirring for 2.8 hours at 53 ℃, filtering the reaction product, and drying for 1.4 hours at 63 ℃ to prepare a mixture of modified nano zirconia and cellulose nano fibers;
(4) Dissolving 5-chloro-2- (2, 4-dichlorophenoxy) phenol in a xylene solution, and stirring for 18min at 64 ℃ to prepare a 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution;
(5) Adding polyvinylidene fluoride-hexafluoropropylene copolymer into polytetrafluoroethylene emulsion, stirring for 33min at 153 ℃, cooling to 64 ℃, adding the mixture of the modified nano zirconia and cellulose nano fiber prepared in the step (3) and the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution prepared in the step (4), stirring and mixing for 43min, and preparing the self-cleaning coating liquid;
(6) Spraying the self-cleaning coating liquid prepared in the step (5) on the glazed ceramic cup prepared in the step (2), and then drying to prepare the self-cleaning glazed ceramic cup.
Wherein:
the ceramic cup blank in the step (1) is composed of the following raw materials in parts by weight: 29 parts of bentonite, 19 parts of cordierite, 16 parts of wollastonite, 10 parts of perlite, 4 parts of fly ash, 8 parts of potassium feldspar, 4 parts of strontium carbonate, 4.5 parts of silicon nitride and 6.5 parts of sepiolite.
The mass of water added during wet ball milling in the step (1) accounts for 30 percent of the sum of the mass of the blank raw material and the mass of water, and the ball milling time is 20 hours.
The drying temperature in the step (1) is 105 ℃ and the drying time is 10 hours.
The pressure of the compression molding in the step (1) is 70MPa.
The glaze layer in the step (2) consists of the following raw materials in parts by weight: 11 parts of nepheline, 9 parts of talcum, 13 parts of sillimanite, 2 parts of calcite, 12 parts of celsian, 7 parts of coal gangue, 14 parts of pyrophyllite, 6 parts of titanium nitride, 7.5 parts of calcium carbide gas powder and 3 parts of titanium diboride.
The slurry in the step (2) is prepared by ball milling the glaze raw material by a wet method and sieving the glaze raw material by a 350-mesh sieve, wherein the mass of added water accounts for 50% of the sum of the mass of water and the glaze raw material.
The drying temperature in the step (2) is 113 ℃, and the drying time is 2.5h.
The firing in the step (2) is performed by heating from room temperature to 555 ℃ for 55min at a heating rate of 8 ℃/min, then heating to 855 ℃ for 50min at a heating rate of 5 ℃/min, and finally heating to 1253 ℃ for 2.1h at a heating rate of 3 ℃/min.
The volume ratio of the absolute ethyl alcohol to the water in the step (3) is 25:1; the volume ratio of perfluorooctyl triethoxysilane to water is 1:1.
In the step (3), the mass sum of the nano zirconia and the cellulose nano fiber and the volume ratio of the nano zirconia to the perfluorooctyl triethoxysilane are 35:8, and the unit is g/mL.
The mass ratio of the nano zirconia to the cellulose nano fiber in the step (3) is 1:0.75.
In the step (4), the mass ratio of the 5-chloro-2- (2, 4-dichlorophenoxy) phenol to the xylene solution is 1:1.
The mass ratio of the polyvinylidene fluoride-hexafluoropropylene copolymer to the polytetrafluoroethylene emulsion in the step (5) is 0.5:1.7.
The mass ratio of the mixture of the modified nano zirconia and the cellulose nano fiber to the polytetrafluoroethylene emulsion in the step (5) is 0.25:1.
The mass ratio of the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution to the polytetrafluoroethylene emulsion in the step (5) is 0.06:1.
In the step (6), the drying temperature is 113 ℃, and the drying time is 6.5 hours.
Example 2
The preparation method of the self-cleaning glazed ceramic cup of the embodiment 2 comprises the following steps:
(1) Uniformly mixing the raw materials of the green body, performing wet ball milling and drying to obtain powder, and performing compression molding on the powder to obtain a ceramic cup green body;
(2) Spreading slurry on the surface of a ceramic cup blank to form a glaze layer, drying and firing, and finally cooling to room temperature at a cooling rate of 10 ℃/h to prepare a glazed ceramic cup;
(3) Adding nano zirconia and cellulose nano fiber into a mixed solution composed of absolute ethyl alcohol and water, stirring for 50min at 50 ℃, then adding sodium hydroxide to adjust the pH value of a reaction system to 8, and continuing stirring for 1.5h; finally, adding perfluorooctyl triethoxysilane, continuously stirring for 3 hours at 50 ℃, filtering the reaction product, and drying for 1.5 hours at 60 ℃ to prepare a mixture of modified nano zirconia and cellulose nano fibers;
(4) Dissolving 5-chloro-2- (2, 4-dichlorophenoxy) phenol in a xylene solution, and stirring for 20min at 62 ℃ to prepare a 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution;
(5) Adding polyvinylidene fluoride-hexafluoropropylene copolymer into polytetrafluoroethylene emulsion, stirring for 35min at 150 ℃, cooling to 62 ℃, adding the mixture of the modified nano zirconia and cellulose nano fiber prepared in the step (3) and the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution prepared in the step (4), stirring and mixing for 45min, and preparing the self-cleaning coating liquid;
(6) Spraying the self-cleaning coating liquid prepared in the step (5) on the glazed ceramic cup prepared in the step (2), and then drying to prepare the self-cleaning glazed ceramic cup.
Wherein:
the ceramic cup blank in the step (1) is composed of the following raw materials in parts by weight: 28 parts of bentonite, 18 parts of cordierite, 17 parts of wollastonite, 9 parts of perlite, 5 parts of fly ash, 9 parts of potassium feldspar, 3 parts of strontium carbonate, 5 parts of silicon nitride and 6 parts of sepiolite.
The mass of water added during wet ball milling in the step (1) accounts for 30 percent of the sum of the mass of the blank raw material and the mass of water, and the ball milling time is 20 hours.
The drying temperature in the step (1) is 105 ℃ and the drying time is 10 hours.
The pressure of the compression molding in the step (1) is 70MPa.
The glaze layer in the step (2) consists of the following raw materials in parts by weight: 10 parts of nepheline, 8 parts of talcum, 12 parts of sillimanite, 3 parts of calcite, 11 parts of celsian, 6 parts of coal gangue, 15 parts of pyrophyllite, 7 parts of titanium nitride, 7 parts of calcium carbide gas powder and 4 parts of titanium diboride.
The slurry in the step (2) is prepared by ball milling the glaze raw material by a wet method and sieving the glaze raw material by a 350-mesh sieve, wherein the mass of added water accounts for 50% of the sum of the mass of water and the glaze raw material.
The drying temperature in the step (2) is 113 ℃, and the drying time is 2.5h.
The firing in the step (2) is performed by heating from room temperature to 550 ℃ for 60min at a heating rate of 8 ℃/min, then heating to 850 ℃ for 55min at a heating rate of 5 ℃/min, and finally heating to 1250 ℃ for 2.2h at a heating rate of 3 ℃/min.
The volume ratio of the absolute ethyl alcohol to the water in the step (3) is 25:1; the volume ratio of perfluorooctyl triethoxysilane to water is 1:1.
In the step (3), the mass sum of the nano zirconia and the cellulose nano fiber and the volume ratio of the nano zirconia to the perfluorooctyl triethoxysilane are 35:8, and the unit is g/mL.
The mass ratio of the nano zirconia to the cellulose nano fiber in the step (3) is 1:0.7.
In the step (4), the mass ratio of the 5-chloro-2- (2, 4-dichlorophenoxy) phenol to the xylene solution is 1:1.
The mass ratio of the polyvinylidene fluoride-hexafluoropropylene copolymer to the polytetrafluoroethylene emulsion in the step (5) is 0.4:1.5.
The mass ratio of the mixture of the modified nano zirconia and the cellulose nano fiber to the polytetrafluoroethylene emulsion in the step (5) is 0.2:1.
The mass ratio of the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution to the polytetrafluoroethylene emulsion in the step (5) is 0.05:1.
In the step (6), the drying temperature is 110 ℃ and the drying time is 7 hours.
Example 3
The preparation method of the self-cleaning glazed ceramic cup in the embodiment 3 comprises the following steps:
(1) Uniformly mixing the raw materials of the green body, performing wet ball milling and drying to obtain powder, and performing compression molding on the powder to obtain a ceramic cup green body;
(2) Spreading slurry on the surface of a ceramic cup blank to form a glaze layer, drying and firing, and finally cooling to room temperature at a cooling rate of 12 ℃/h to prepare a glazed ceramic cup;
(3) Adding nano zirconia and cellulose nano fiber into a mixed solution composed of absolute ethyl alcohol and water, stirring for 45min at 55 ℃, then adding sodium hydroxide to adjust the pH value of a reaction system to 8, and continuing stirring for 1.7h; finally adding perfluorooctyl triethoxysilane, continuously stirring for 2.5 hours at 55 ℃, filtering the reaction product, and drying for 1.2 hours at 65 ℃ to prepare a mixture of modified nano zirconia and cellulose nano fibers;
(4) Dissolving 5-chloro-2- (2, 4-dichlorophenoxy) phenol in a xylene solution, and stirring for 15min at 65 ℃ to prepare a 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution;
(5) Adding polyvinylidene fluoride-hexafluoropropylene copolymer into polytetrafluoroethylene emulsion, stirring for 30min at 155 ℃, cooling to 65 ℃, adding the mixture of the modified nano zirconia and cellulose nano fiber prepared in the step (3) and the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution prepared in the step (4), stirring and mixing for 40min, and preparing the self-cleaning coating liquid;
(6) Spraying the self-cleaning coating liquid prepared in the step (5) on the glazed ceramic cup prepared in the step (2), and then drying to prepare the self-cleaning glazed ceramic cup.
Wherein:
the ceramic cup blank in the step (1) is composed of the following raw materials in parts by weight: 30 parts of bentonite, 20 parts of cordierite, 15 parts of wollastonite, 11 parts of perlite, 3 parts of fly ash, 7 parts of potassium feldspar, 5 parts of strontium carbonate, 4 parts of silicon nitride and 7 parts of sepiolite.
The mass of water added during wet ball milling in the step (1) accounts for 30 percent of the sum of the mass of the blank raw material and the mass of water, and the ball milling time is 20 hours.
The drying temperature in the step (1) is 105 ℃ and the drying time is 10 hours.
The pressure of the compression molding in the step (1) is 70MPa.
The glaze layer in the step (2) consists of the following raw materials in parts by weight: 12 parts of nepheline, 10 parts of talcum, 14 parts of sillimanite, 1 part of calcite, 13 parts of celsian, 8 parts of coal gangue, 13 parts of pyrophyllite, 5 parts of titanium nitride, 8 parts of calcium carbide gas powder and 2 parts of titanium diboride.
The slurry in the step (2) is prepared by ball milling the glaze raw material by a wet method and sieving the glaze raw material by a 350-mesh sieve, wherein the mass of added water accounts for 50% of the sum of the mass of water and the glaze raw material.
The drying temperature in the step (2) is 113 ℃, and the drying time is 2.5h.
The firing in the step (2) is performed by heating from room temperature to 560 ℃ for 50min at a heating rate of 8 ℃/min, then heating to 860 ℃ at a heating rate of 5 ℃/min for 45min, and finally heating to 1255 ℃ at a heating rate of 3 ℃/min for 2.0 h.
The volume ratio of the absolute ethyl alcohol to the water in the step (3) is 25:1; the volume ratio of perfluorooctyl triethoxysilane to water is 1:1.
In the step (3), the mass sum of the nano zirconia and the cellulose nano fiber and the volume ratio of the nano zirconia to the perfluorooctyl triethoxysilane are 35:8, and the unit is g/mL.
In the step (3), the mass ratio of the nano zirconia to the cellulose nano fiber is 1:0.8.
In the step (4), the mass ratio of the 5-chloro-2- (2, 4-dichlorophenoxy) phenol to the xylene solution is 1:1.
The mass ratio of the polyvinylidene fluoride-hexafluoropropylene copolymer to the polytetrafluoroethylene emulsion in the step (5) is 0.6:1.8.
The mass ratio of the mixture of the modified nano zirconia and the cellulose nano fiber to the polytetrafluoroethylene emulsion in the step (5) is 0.3:1.
The mass ratio of the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution to the polytetrafluoroethylene emulsion in the step (5) is 0.08:1.
In the step (6), the drying temperature is 115 ℃ and the drying time is 6 hours.
Comparative example 1
The preparation method of the self-cleaning glazed ceramic cup in the comparative example 1 is the same as that in the example 1, and the only difference is that the raw materials of the green body in the step (1) are different, and the ceramic cup green body in the step (1) in the comparative example 1 is composed of the following raw materials in parts by weight: 29 parts of bentonite, 19 parts of cordierite, 16 parts of wollastonite, 10 parts of perlite, 4 parts of fly ash and 8 parts of potassium feldspar.
Comparative example 2
The preparation method of the self-cleaning glazed ceramic cup in the comparative example 2 is the same as that in the example 1, and the only difference is that the glaze layer in the step (2) is different in raw materials, and the glaze layer in the step (2) consists of the following raw materials in parts by weight: 11 parts of nepheline, 9 parts of talcum, 13 parts of sillimanite, 2 parts of calcite, 12 parts of celsian and 7 parts of coal gangue.
Comparative example 3
The preparation method of the self-cleaning glazed ceramic cup in the comparative example 3 is the same as that in the example 1, and the only difference is that the self-cleaning coating liquid in the step (5) is different, and the preparation method of the self-cleaning coating liquid in the step (5) is as follows: adding polyvinylidene fluoride-hexafluoropropylene copolymer into polytetrafluoroethylene emulsion, stirring for 33min at 153 ℃, cooling to 64 ℃, adding the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution prepared in the step (4), stirring and mixing for 43min, and obtaining the self-cleaning coating liquid.
The self-cleaning glazed ceramic cups prepared in examples 1-3 and comparative examples 1-3 were subjected to performance tests, the results of which are shown in Table 1 below:
the prepared self-cleaning ceramic tile was subjected to performance test according to GB/T3810-2016 ceramic tile test method (stain resistance grade according to GB/T3810.14-2016; family chemical resistance and swimming pool salt corrosion grade according to GB/T3810.13-2016; breaking strength according to GB/T3810.4-2016; frictional wear test on MMS-1G high speed pin plate frictional wear tester, and abrasion amount recorded), and the results are shown in Table 1 below:
table 1 ceramic tile performance test results
Claims (10)
1. A preparation method of a self-cleaning glazed ceramic cup is characterized by comprising the following steps: the method comprises the following steps:
(1) Uniformly mixing the raw materials of the green body, performing wet ball milling and drying to obtain powder, and performing compression molding on the powder to obtain a ceramic cup green body;
(2) Spreading slurry on the surface of a ceramic cup blank to form a glaze layer, drying and firing, and finally cooling to room temperature at a cooling rate of 10-12 ℃/h to prepare a glazed ceramic cup;
(3) Adding nano zirconia and cellulose nano fiber into a mixed solution composed of absolute ethyl alcohol and water, stirring for 45-50min at 50-55 ℃, then adding sodium hydroxide to adjust the pH value of a reaction system to 8, and continuing stirring for 1.5-1.7h; finally adding perfluorooctyl triethoxysilane, continuously stirring for 2.5-3 hours at 50-55 ℃, filtering the reaction product, and drying for 1.2-1.5 hours at 60-65 ℃ to prepare a mixture of modified nano zirconia and cellulose nano fibers;
(4) Dissolving 5-chloro-2- (2, 4-dichlorophenoxy) phenol in a xylene solution, and stirring for 15-20min at 62-65 ℃ to prepare a 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution;
(5) Adding polyvinylidene fluoride-hexafluoropropylene copolymer into polytetrafluoroethylene emulsion, stirring for 30-35min at 150-155 ℃, cooling to 62-65 ℃, adding the mixture of modified nano zirconia and cellulose nano fiber prepared in the step (3) and the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution prepared in the step (4), stirring and mixing for 40-45min, and preparing the self-cleaning coating liquid;
(6) Spraying the self-cleaning coating liquid prepared in the step (5) on the glazed ceramic cup prepared in the step (2), and then drying to prepare the self-cleaning glazed ceramic cup.
2. The method for preparing the self-cleaning glazed ceramic cup according to claim 1, which is characterized in that: the ceramic cup blank in the step (1) is composed of the following raw materials in parts by weight: 28-30 parts of bentonite, 18-20 parts of cordierite, 15-17 parts of wollastonite, 9-11 parts of perlite, 3-5 parts of fly ash, 7-9 parts of potassium feldspar, 3-5 parts of strontium carbonate, 4-5 parts of silicon nitride and 6-7 parts of sepiolite.
3. The method for preparing the self-cleaning glazed ceramic cup according to claim 1, which is characterized in that: the mass of water added during wet ball milling in the step (1) accounts for 30 percent of the sum of the mass of the blank raw material and the mass of water, and the ball milling time is 20 hours;
the drying temperature in the step (1) is 105 ℃, and the drying time is 10 hours;
the pressure of the compression molding in the step (1) is 70MPa.
4. The method for preparing the self-cleaning glazed ceramic cup according to claim 1, which is characterized in that: the glaze layer in the step (2) consists of the following raw materials in parts by weight: 10-12 parts of nepheline, 8-10 parts of talcum, 12-14 parts of sillimanite, 1-3 parts of calcite, 11-13 parts of celsian, 6-8 parts of coal gangue, 13-15 parts of pyrophyllite, 5-7 parts of titanium nitride, 7-8 parts of calcium carbide gas powder and 2-4 parts of titanium diboride.
5. The method for preparing the self-cleaning glazed ceramic cup according to claim 1, which is characterized in that: the slurry in the step (2) is prepared by ball milling the glaze raw material by a wet method and sieving the glaze raw material by a 350-mesh sieve, wherein the mass of added water accounts for 50% of the sum of the mass of water and the glaze raw material;
the drying temperature in the step (2) is 113 ℃, and the drying time is 2.5h;
the firing in the step (2) is carried out by heating from room temperature to 550-560 ℃ for 50-60min at a heating rate of 8 ℃/min, then heating to 850-860 ℃ for 45-55min at a heating rate of 5 ℃/min, and finally heating to 1250-1255 ℃ for 2-2.2h at a heating rate of 3 ℃/min.
6. The method for preparing the self-cleaning glazed ceramic cup according to claim 1, which is characterized in that: the volume ratio of the absolute ethyl alcohol to the water in the step (3) is 25:1; the volume ratio of the perfluorooctyl triethoxysilane to the water is 1:1;
in the step (3), the mass sum of the nano zirconia and the cellulose nano fiber and the volume ratio of the nano zirconia to the perfluorooctyl triethoxysilane are 35:8, and the unit is g/mL;
in the step (3), the mass ratio of the nano zirconia to the cellulose nano fiber is 1:0.7-0.8.
7. The method for preparing the self-cleaning glazed ceramic cup according to claim 1, which is characterized in that: in the step (4), the mass ratio of the 5-chloro-2- (2, 4-dichlorophenoxy) phenol to the xylene solution is 1:1.
8. The method for preparing the self-cleaning glazed ceramic cup according to claim 1, which is characterized in that: the mass ratio of the polyvinylidene fluoride-hexafluoropropylene copolymer to the polytetrafluoroethylene emulsion in the step (5) is 0.4-0.6:1.5-1.8;
the mass ratio of the mixture of the modified nano zirconia and the cellulose nano fiber to the polytetrafluoroethylene emulsion in the step (5) is 0.2-0.3:1.
9. The method for preparing the self-cleaning glazed ceramic cup according to claim 1, which is characterized in that: in the step (5), the mass ratio of the 5-chloro-2- (2, 4-dichlorophenoxy) phenol solution to the polytetrafluoroethylene emulsion is 0.05-0.08:1.
10. The method for preparing the self-cleaning glazed ceramic cup according to claim 1, which is characterized in that: in the step (6), the drying temperature is 110-115 ℃ and the drying time is 6-7h.
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