CN112661494A - Composite antibacterial ceramic tile and preparation process thereof - Google Patents
Composite antibacterial ceramic tile and preparation process thereof Download PDFInfo
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- CN112661494A CN112661494A CN202011573181.9A CN202011573181A CN112661494A CN 112661494 A CN112661494 A CN 112661494A CN 202011573181 A CN202011573181 A CN 202011573181A CN 112661494 A CN112661494 A CN 112661494A
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 71
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000010434 nepheline Substances 0.000 claims abstract description 49
- 229910052664 nepheline Inorganic materials 0.000 claims abstract description 49
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- 229910052623 talc Inorganic materials 0.000 claims abstract description 45
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- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 37
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- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 34
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- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000010433 feldspar Substances 0.000 claims abstract description 32
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- 239000006004 Quartz sand Substances 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 56
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 54
- 238000000034 method Methods 0.000 claims description 51
- 238000000227 grinding Methods 0.000 claims description 38
- 229910052845 zircon Inorganic materials 0.000 claims description 35
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 35
- 239000001095 magnesium carbonate Substances 0.000 claims description 34
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 34
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 34
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 34
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 claims description 30
- 229910052642 spodumene Inorganic materials 0.000 claims description 30
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 27
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- 239000000843 powder Substances 0.000 claims description 26
- 230000008569 process Effects 0.000 claims description 26
- 238000007873 sieving Methods 0.000 claims description 26
- 239000002994 raw material Substances 0.000 claims description 25
- 238000001694 spray drying Methods 0.000 claims description 22
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- 239000005751 Copper oxide Substances 0.000 claims description 21
- 229910000431 copper oxide Inorganic materials 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 229910021389 graphene Inorganic materials 0.000 claims description 19
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
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- 238000005342 ion exchange Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
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- 238000000465 moulding Methods 0.000 claims description 8
- 238000004806 packaging method and process Methods 0.000 claims description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 239000004115 Sodium Silicate Substances 0.000 claims description 6
- 238000007688 edging Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
- 239000000126 substance Substances 0.000 abstract description 2
- 235000012222 talc Nutrition 0.000 abstract 1
- 239000002002 slurry Substances 0.000 description 16
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- VNSBYDPZHCQWNB-UHFFFAOYSA-N calcium;aluminum;dioxido(oxo)silane;sodium;hydrate Chemical compound O.[Na].[Al].[Ca+2].[O-][Si]([O-])=O VNSBYDPZHCQWNB-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a composite antibacterial ceramic tile and a preparation process thereof, wherein the antibacterial ceramic tile is composed of the following components in parts by weight: 20 to 45 percent of quartz sand, 15 to 20 percent of kaolin, 5 to 7 percent of feldspar, 5 to 7 percent of copper nitrate, 8 to 10 percent of wollastonite, 1 to 2 percent of talcum, 5 to 7 percent of nepheline, 5 to 8 percent of antibacterial agent, 6 to 9 percent of auxiliary material and 5 to 10 percent of reinforcing material. The preparation process of the composite antibacterial ceramic tile provided by the invention can automatically release the glaze in the manufacturing process of the ceramic tile, and can automatically release part of antibacterial substances to the ceramic tile on the outer layer of the ceramic tile by utilizing the self-release glaze so as to realize long-acting antibacterial.
Description
Technical Field
The invention relates to the technical field of building ceramic materials, in particular to a composite antibacterial ceramic tile and a preparation process thereof.
Background
The ceramic tile is a plate-shaped or block-shaped ceramic product produced by clay and other inorganic non-metallic raw materials through processes of molding, sintering and the like, and can be used for decorating and protecting wall surfaces and ground surfaces of buildings and structures. In practical application, due to the application of some special scenes, some ceramic tiles with special functions are needed to meet the requirements of practical application. For example, in some special places such as hospitals and pharmacies, floor tiles with long-acting antibacterial function are required to meet the practical application requirements.
The prior patent (application number: CN201410334157.8) provides a bacteriostatic and deodorant ceramic tile and a preparation method thereof, and the product comprises the following components in parts by weight: 80-100 parts of zircon sand, 40-60 parts of volcanic mud, 35-55 parts of beidellite, 28-36 parts of coal cinder, 20-30 parts of magnetic wave stone, 15-25 parts of calcite, 12-18 parts of corundum powder, 10-15 parts of ball clay, 14-26 parts of mung bean rock, 20-25 parts of sepiolite, 30-40 parts of crushed gravel, 10-15 parts of nano calcium titanate, 15-20 parts of blast furnace slag, 5-10 parts of Chinese medicine residue ash and 18-27 parts of waste glass powder. The product has broad-spectrum antibacterial effect, and has effects of absorbing polluted gases such as toluene and formaldehyde.
The products in the patent have the characteristic of broad-spectrum antibiosis, and can absorb decorative pollution gases such as toluene, formaldehyde and the like. However, the ceramic tile has short antibacterial effectiveness and long production period, and cannot well meet the requirements of practical application in some occasions. Therefore, a new ceramic tile with long-lasting antibacterial function is needed.
Disclosure of Invention
Based on the above, the invention aims to provide a composite antibacterial ceramic tile and a preparation process thereof, which are used for solving the technical problems in the background technology.
The invention provides a composite antibacterial ceramic tile which comprises the following components in percentage by weight: 20-45% of quartz sand, 15-20% of kaolin, 5-7% of feldspar, 5-7% of copper nitrate, 8-10% of wollastonite, 1-2% of talc, 5-7% of nepheline, 5-8% of an antibacterial agent, 6-9% of auxiliary materials and 5-10% of reinforcing materials, wherein the auxiliary materials comprise zircon, magnesite and spodumene, the antibacterial agent comprises bentonite and silver nitrate, and the reinforcing materials comprise carbon nitride and graphene.
Preferably, the auxiliary materials comprise the following components in percentage by weight:
zircon 2% -3%, magnesite 2% -3% and spodumene 2% -3%. In the preferred embodiment, magnesite and zircon are particularly well refractory, and spodumene acts as a flux while ensuring the formation of the essential components of low thermal expansion crystals.
Preferably, the antibacterial agent comprises the following components in percentage by weight:
3 to 5 percent of bentonite and 2 to 3 percent of silver nitrate. In the preferred embodiment, the bentonite and the silver nitrate can generate the nano silver-loaded inorganic antibacterial agent taking the bentonite as the carrier, and the nano silver-loaded inorganic antibacterial agent has lasting antibacterial effect and is green and environment-friendly.
Preferably, the reinforcing material comprises the following components in percentage by weight:
2 to 6 percent of carbon nitride and 3 to 4 percent of graphene. In the preferred embodiment, the carbon nitride has high strength, the graphene has excellent properties such as toughness, and the carbon nitride and the graphene are combined to greatly increase the strength of the ceramic tile.
Preferably, the composite antibacterial ceramic tile comprises the following components in percentage by weight:
35% of quartz sand, 15% of kaolin, 5% of feldspar, 5% of copper nitrate, 10% of wollastonite, 1% of talc, 5% of nepheline, 3% of zircon, 3% of magnesite, 3% of spodumene, 3% of bentonite, 2% of silver nitrate, 6% of carbon nitride and 4% of graphene. In the preferred embodiment, the kaolin renders the dry green malleable since the silica sand is the skeletal material in the ceramic tile. The feldspar plays a role of a 'fluxing agent', the magnesite and the zircon have excellent fire resistance, copper nitrate generates copper oxide in the processing process and has specific antibacterial property, and wollastonite, nepheline and talc are matched to generate a self-releasing glaze phenomenon in the firing process. The bentonite has plasticity and can generate a nano silver-carrying inorganic antibacterial agent taking the bentonite as a carrier with silver nitrate, so that the ceramic tile prepared by the formula has good fire-resistant effect, poor antibacterial effect, better glaze glossiness and high strength.
Preferably, the composite antibacterial ceramic tile comprises the following components in percentage by weight:
30% of quartz sand, 20% of kaolin, 5% of feldspar, 7% of copper nitrate, 10% of wollastonite, 1% of talc, 5% of nepheline, 3% of zircon, 3% of magnesite, 3% of spodumene, 5% of bentonite, 3% of silver nitrate, 2% of carbon nitride and 3% of graphene. In the preferred embodiment, because the quartz sand is the framework material in the ceramic tile, the kaolin endows the dry blank with plasticity, the feldspar plays the role of a 'fluxing agent', the magnesite and the zircon have excellent fire resistance, the copper nitrate generates copper oxide during the processing process and has specific antibacterial property, and the wollastonite, nepheline and talc are matched to generate the self-releasing glaze phenomenon during the firing process. The bentonite has plasticity and can generate a nano silver-loaded inorganic antibacterial agent taking the bentonite as a carrier with silver nitrate, so that the ceramic tile prepared by the formula has good fire-resistant effect, good antibacterial effect, better glaze glossiness and general strength.
Preferably, the composite antibacterial ceramic tile comprises the following components in percentage by weight:
20% of quartz sand, 20% of kaolin, 7% of feldspar, 7% of copper nitrate, 10% of wollastonite, 2% of talc, 7% of nepheline, 3% of zircon, 3% of magnesite, 3% of spodumene, 5% of bentonite, 3% of silver nitrate, 6% of carbon nitride and 4% of graphene. In the preferred embodiment, because the quartz sand is the framework material in the ceramic tile, the kaolin endows the dry blank with plasticity, the feldspar plays the role of a 'fluxing agent', the magnesite and the zircon have excellent fire resistance, the copper nitrate generates copper oxide during the processing process and has specific antibacterial property, and the wollastonite, nepheline and talc are matched to generate the self-releasing glaze phenomenon during the firing process. The bentonite has plasticity and can generate a nano silver-loaded inorganic antibacterial agent taking the bentonite as a carrier with silver nitrate, so that the ceramic tile prepared by the formula has good fire resistance, good antibacterial effect, good glaze glossiness and high strength.
The invention also provides a preparation process of the composite antibacterial ceramic tile, which is used for preparing the composite antibacterial ceramic tile, and the method comprises the following steps:
the method comprises the following steps: preparing bentonite and silver nitrate according to the formula amount, and preparing a nano silver-loaded inorganic antibacterial agent taking the bentonite as a carrier by adopting an ion exchange method for later use;
step two: taking kaolin, feldspar, quartz sand, zircon, magnesite, spodumene and copper nitrate according to the formula ratio, uniformly mixing the raw materials, and adding the mixture into a ball mill for grinding for 8-10 hours; wherein the ratio of the added raw materials, the grinding balls and water is 1: 0.8: 0.5, the mixture is sieved by a 100-150-mesh sieve after grinding is finished, spray drying is carried out at the hot air temperature of 450-500 ℃ after sieving, most of nitric acid in copper nitrate is removed in the spray drying process, and the mixed powder I is obtained by drying and collecting powder;
step three: crushing nepheline, talc and wollastonite according to the formula amount, sieving the crushed nepheline, talc and wollastonite with a 200-300-mesh sieve, adding the crushed nepheline, talc and wollastonite and the mixed powder I into a stirrer, adding sodium silicate with the solid content of 35 percent, which is 3-7 percent of the weight of the mixture, stirring and mixing for 20min, adding a nano silver-loaded inorganic antibacterial agent with bentonite as a carrier, carbon nitride and graphene, stirring for 20-30 min again, pressing and molding powder under the pressure of 30-40MPa after stirring, and drying for 3-4 h at the temperature of 60-70 ℃ to prepare a dry blank;
step four: raising the temperature of the prepared dry blank to 850-900 ℃ at a heating rate of 10-15 ℃/min, preserving heat for 1-2 h, decomposing copper oxide by the copper removed by nitric acid at high temperature, raising the temperature to 1200-1300 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 3-4 h, melting and releasing the copper oxide to the surface of the blank at the raising temperature due to the low melting point of nepheline, driving part of the copper oxide and the nano silver-loaded inorganic antibacterial agent taking bentonite as a carrier to move outwards, reducing the temperature to 340-380 ℃ at a cooling rate of 6-8 ℃/min, preserving heat for 2-3 h, cooling to normal temperature, edging, and packaging to obtain the finished product.
The preparation process of the composite antibacterial ceramic tile adopts an ion exchange method to carry out reaction under the conditions that the temperature is 120 ℃, the pH value is less than 7 and the reaction time is 24 hours. In the preferred embodiment, the control of temperature, pH and time is used to facilitate the sufficient valence bond binding of silver ions in the pores of the bentonite.
According to the preparation process of the composite antibacterial ceramic tile, after the preparation of the dry blank is finished, printing treatment is carried out on the dry blank. In the present preferred embodiment, the tile may be given a different finish by the printing process.
Compared with the prior art, the invention has the beneficial effects that:
(1) the quartz sand is a framework material in the ceramic tile, the kaolin enables the dry blank to have plasticity, and the feldspar plays a role of a fluxing agent. The bentonite and the silver nitrate are adopted to generate the nano silver-loaded inorganic antibacterial agent which takes the bentonite as a carrier, the antibacterial property is lasting, the environment is protected, the plasticity of the bentonite enables a dry blank to be easily molded, and the copper nitrate in the formula generates copper oxide in the processing process and has the antibacterial property;
(2) the combination of wollastonite, nepheline and talc can generate a self-releasing glaze phenomenon in the firing process, and the processing steps of preparing and applying the glaze are omitted. In addition, in the process of melting and releasing nepheline, partial copper oxide and the nano silver-loaded inorganic antibacterial substance taking bentonite as a carrier are driven to move outwards, so that the antibacterial effect of the surface of the ceramic tile is better.
Additional features and advantages of the disclosure will be set forth in the description which follows, or in part may be learned by the practice of the above-described techniques of the disclosure, or may be learned by practice of the disclosure.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
FIG. 1 is a flow chart of the preparation process of the composite antibacterial ceramic tile provided by the invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1:
the first embodiment of the invention provides a composite antibacterial ceramic tile, which comprises the following components in parts by weight: 35% of quartz sand, 15% of kaolin, 5% of feldspar, 5% of copper nitrate, 10% of wollastonite, 1% of talc, 5% of nepheline, 3% of zircon, 3% of magnesite, 3% of spodumene, 3% of bentonite, 2% of silver nitrate, 6% of carbon nitride and 4% of graphene.
In the embodiment, a preparation process of a composite antibacterial ceramic tile is correspondingly provided, which comprises the following steps:
the method comprises the following steps: taking bentonite and silver nitrate according to the formula amount, and preparing a nano silver-loaded inorganic antibacterial agent taking the bentonite as a carrier by adopting an ion exchange method for standby, wherein the reaction condition of the ion exchange method is that the temperature is 120 ℃, the pH value is less than 7 during the reaction, and the reaction time is 24 hours;
step two: taking kaolin, feldspar, quartz sand, zircon, magnesite, spodumene and copper nitrate according to the formula ratio, uniformly mixing the raw materials, adding the raw materials into a ball mill, grinding for 8-10 h, wherein the ratio of the raw materials to grinding balls to water is 1: 0.8: 0.5, sieving by a 100-150-mesh sieve after grinding, carrying out spray drying after sieving, removing most of nitric acid in the copper nitrate in the spray drying process at the hot air temperature of 500 ℃, and collecting dried powder to obtain mixed powder I;
step three: crushing nepheline, talc and wollastonite according to the formula amount, sieving with a 200-300-mesh sieve, adding the crushed nepheline, talc and wollastonite and the mixed powder I into a stirrer, adding sodium silicate with solid content of 35% which is 3-7% of the weight of the mixture, stirring and mixing for 20min, adding a nano silver-loaded inorganic antibacterial agent with bentonite as a carrier, stirring for 20-30 min again, pressing and molding powder under the pressure of 30-40MPa after stirring, drying at 60-70 ℃ for 3-4 h to prepare a dry blank, and performing printing treatment after the dry blank is finished;
step four: raising the temperature of the prepared dry blank to 850-900 ℃ at the heating rate of 10-15 ℃/min, and preserving the temperature for 1-2 h, wherein copper removed by nitric acid is subjected to pyrolysis copper oxide; raising the temperature to 1200-1300 ℃ at a heating rate of 5-10 ℃/min and preserving the heat for 3-4 h; when the temperature is raised, the nepheline is melted and released to the surface of the blank firstly due to low melting point of the nepheline, and part of the copper oxide and the nano silver-loaded inorganic antibacterial agent taking the bentonite as a carrier are driven to move outwards, then the temperature is reduced to 340-380 ℃ at the cooling rate of 6-8 ℃/min, the temperature is kept for 2-3 h, the temperature is cooled to the normal temperature, and the finished product is obtained after edge grinding and packaging.
Example 2:
the second embodiment of the invention provides a composite antibacterial ceramic tile, which comprises the following components in parts by weight:
30% of quartz sand, 20% of kaolin, 5% of feldspar, 7% of copper nitrate, 10% of wollastonite, 1% of talc, 5% of nepheline, 3% of zircon, 3% of magnesite, 3% of spodumene, 5% of bentonite, 3% of silver nitrate, 2% of carbon nitride and 3% of graphene.
In the embodiment, a preparation process of a composite antibacterial ceramic tile is correspondingly provided, which comprises the following steps:
the method comprises the following steps: taking bentonite and silver nitrate according to the formula amount, and preparing a nano silver-loaded inorganic antibacterial agent taking the bentonite as a carrier by adopting an ion exchange method for standby, wherein the reaction condition of the ion exchange method is that the temperature is 120 ℃, the pH value is less than 7 during the reaction, and the reaction time is 24 hours;
step two: taking kaolin, feldspar, quartz sand, zircon, magnesite, spodumene and copper nitrate according to the formula ratio, uniformly mixing the raw materials, adding the raw materials into a ball mill, grinding for 8 hours, wherein the ratio of the raw materials to grinding balls to water is 1: 0.8: 0.5, sieving by a 100-mesh sieve after grinding is finished, carrying out spray drying after sieving, carrying out hot air temperature of 500 ℃, removing most of nitric acid in the copper nitrate in the spray drying process, and collecting dried powder to obtain mixed powder I;
step three: crushing nepheline, talc and wollastonite according to the formula, sieving by a 200-mesh sieve, adding the crushed nepheline, talc and wollastonite and the mixed powder I into a stirrer, adding sodium silicate with the solid content of 35 percent and the weight of 3 percent of the mixture into the stirrer, stirring and mixing the mixture for 20min, adding a nano silver-loaded inorganic antibacterial agent with bentonite as a carrier, stirring the mixture for 20min again, pressing and molding powder under the pressure of 30MPa after stirring, drying the powder for 3h at 70 ℃ to prepare a dry blank, and printing the dry blank after finishing;
step four: raising the temperature of the prepared dry blank to 900 ℃ at the heating rate of 15 ℃/min, and preserving the temperature for 1h, wherein copper removed by nitric acid is subjected to pyrolysis to oxidize copper; raising the temperature to 1200 ℃ at the heating rate of 5 ℃/min and preserving the heat for 3 hours; when the temperature is raised, the nepheline is melted and released to the surface of the blank body firstly due to low melting point of the nepheline, and part of the copper oxide and the nano silver-loaded inorganic antibacterial agent taking the bentonite as the carrier are driven to move outwards, then the temperature is reduced to 340 ℃ at the cooling rate of 6 ℃/min and is kept for 2 hours, and the product is obtained after cooling to the normal temperature, edging and packaging.
Example 3:
the third embodiment of the invention provides a composite antibacterial ceramic tile, which comprises the following components in parts by weight:
20% of quartz sand, 20% of kaolin, 7% of feldspar, 7% of copper nitrate, 10% of wollastonite, 2% of talc, 7% of nepheline, 3% of zircon, 3% of magnesite, 3% of spodumene, 5% of bentonite, 3% of silver nitrate, 6% of carbon nitride and 4% of graphene.
In the embodiment, a preparation process of a composite antibacterial ceramic tile is correspondingly provided, which comprises the following steps:
the method comprises the following steps: taking bentonite and silver nitrate according to the formula amount, and preparing a nano silver-loaded inorganic antibacterial agent taking the bentonite as a carrier by adopting an ion exchange method for standby, wherein the reaction condition of the ion exchange method is that the temperature is 120 ℃, the pH value is less than 7 during the reaction, and the reaction time is 24 hours;
step two: taking kaolin, feldspar, quartz sand, zircon, magnesite, spodumene and copper nitrate according to the formula ratio, uniformly mixing the raw materials, adding the raw materials into a ball mill, and grinding for 8 hours, wherein the ratio of the raw materials to grinding balls to water is 1: 0.8: 0.5, after grinding, sieving the mixture by a 100-mesh sieve, and then carrying out spray drying at the hot air temperature of 500 ℃, removing most of nitric acid in the copper nitrate in the spray drying process, and collecting dried powder to obtain mixed powder I;
step three: crushing nepheline, talc and wollastonite according to the formula, sieving the crushed nepheline, talc and wollastonite with a 300-mesh sieve, adding the crushed nepheline, talc and wollastonite and the mixed powder I into a stirrer, adding water glass with the solid content of 35 percent and the weight of 7 percent of the mixture, stirring and mixing for 20min, adding a nano silver-loaded inorganic antibacterial agent with bentonite as a carrier, stirring for 30min again, after stirring, pressing and molding powder under the pressure of 40MPa, drying for 4h at 70 ℃ to prepare a dry blank, and after the dry blank is finished, carrying out printing treatment;
step four: raising the temperature of the prepared dry blank to 900 ℃ at the heating rate of 15 ℃/min, and preserving the temperature for 2h, wherein copper removed by nitric acid is subjected to high-temperature decomposition to form copper oxide; then rising to 1300 ℃ at the heating rate of 10 ℃/min and preserving the heat for 4 h; when the temperature is raised, the nepheline is melted and released to the surface of the blank body firstly due to low melting point of the nepheline, and part of the copper oxide and the nano silver-loaded inorganic antibacterial agent taking the bentonite as the carrier are driven to move outwards, then the temperature is reduced to 380 ℃ at the cooling rate of 8 ℃/min and is kept for 3 hours, the temperature is cooled to the normal temperature, and the finished product is obtained after edging and packaging.
Example 4:
the fourth embodiment of the invention provides a composite antibacterial ceramic tile, which comprises the following components in parts by weight:
35% of quartz sand, 20% of kaolin, 7% of feldspar, 5% of copper nitrate, 8% of wollastonite, 1% of talc, 5% of nepheline, 2% of zircon, 2% of magnesite, 2% of spodumene, 4% of bentonite, 2% of silver nitrate, 3% of carbon nitride and 4% of graphene.
In the embodiment, a preparation process of a composite antibacterial ceramic tile is correspondingly provided, which comprises the following steps:
the method comprises the following steps: taking bentonite and silver nitrate according to the formula amount, and preparing a nano silver-loaded inorganic antibacterial agent taking the bentonite as a carrier by adopting an ion exchange method for standby, wherein the reaction condition of the ion exchange method is that the temperature is 120 ℃, the pH value is less than 7 during the reaction, and the reaction time is 24 hours;
step two: taking kaolin, feldspar, quartz sand, zircon, magnesite, spodumene and copper nitrate according to the formula ratio, uniformly mixing the raw materials, adding the raw materials into a ball mill, grinding for 9 hours, wherein the ratio of the raw materials to grinding balls to water is 1: 0.8: 0.5, sieving by a 125-mesh sieve after grinding is finished, carrying out spray drying after sieving, removing most nitric acid in the copper nitrate in the spray drying process at the hot air temperature of 450 ℃, and collecting dried powder to obtain mixed powder I;
step three: crushing nepheline, talc and wollastonite according to the formula, sieving the crushed nepheline, talc and wollastonite with a 300-mesh sieve, adding the crushed nepheline, talc and wollastonite and the mixed powder I into a stirrer, adding sodium silicate with solid content of 35 percent and the weight of 3-7 percent of the weight of the mixture, stirring and mixing for 20min, adding a nano silver-loaded inorganic antibacterial agent with bentonite as a carrier, stirring for 30min again, pressing and molding powder under the pressure of 35MPa after stirring, drying for 4h at 65 ℃ to prepare a dry blank, and printing the dry blank after finishing;
step four: raising the temperature of the prepared dry blank to 900 ℃ at the heating rate of 15 ℃/min, and preserving the temperature for 2h, wherein copper removed by nitric acid is subjected to high-temperature decomposition to form copper oxide; then rising to 1300 ℃ at the heating rate of 10 ℃/min and preserving the heat for 4 h; when the temperature is raised, the nepheline is melted and released to the surface of the blank firstly due to low melting point of the nepheline, and part of the copper oxide and the nano silver-loaded inorganic antibacterial agent taking bentonite as a carrier are driven to move outwards, then the temperature is reduced to 380 ℃ at the cooling rate of 6-8 ℃/min, the temperature is kept for 3 hours, the temperature is cooled to the normal temperature, and the finished product is obtained after edging and packaging.
Example 5:
the fifth embodiment of the invention provides a ceramic tile, which consists of the following components in percentage by weight:
35% of quartz sand, 20% of kaolin, 5% of feldspar, 1% of talc, 3% of zircon, 3% of magnesite and 2% of spodumene.
In this embodiment, a process for preparing a ceramic tile is provided, which includes the following steps:
the method comprises the following steps: feeding and grinding, namely adding the weighed quartz sand, kaolin, feldspar, talc, zircon, magnesite and spodumene into a ball mill for grinding for 10-12 h, wherein the ratio of raw materials, grinding balls and water is 1: 0.8, and preparing slurry I after grinding is finished;
step two: sieving and ageing, namely sieving the first slurry to remove iron, putting the first slurry into a slurry tank, and ageing for 8-10 hours to obtain a first mixed slurry after ageing is finished;
step three: spray drying, namely spray drying the mixed slurry I at the hot air temperature of 500 ℃ to obtain powder I;
step four: and (3) forming, wherein the pressure is controlled to be 20-30 MPa, the powder is pressed and formed, then the powder is dried for 4-6 hours at 50-60 ℃, the dried product is placed in a firing furnace, the temperature is controlled to be 1200-1300 ℃, the firing is carried out for 1-2 hours, and the ceramic product is obtained after the mould inversion and cooling.
Example 6:
the sixth embodiment of the invention provides a ceramic tile, which consists of the following components in percentage by weight:
33% of quartz sand, 20% of kaolin, 5% of feldspar, 2% of talc, 2% of zircon, 3% of magnesite and 3% of spodumene.
In this embodiment, a process for preparing a ceramic tile is provided, which includes the following steps:
the method comprises the following steps: feeding and grinding, namely adding the weighed quartz sand, kaolin, feldspar, talc, zircon, magnesite and spodumene into a ball mill for grinding for 12 hours, wherein the ratio of raw materials, grinding balls and water is 1: 0.8, and preparing slurry I after grinding is finished;
step two: sieving and ageing, namely sieving the first slurry to remove iron, putting the first slurry into a slurry tank, and ageing for 10 hours to obtain first mixed slurry after ageing is finished;
step three: spray drying, namely spray drying the mixed slurry I at the hot air temperature of 500 ℃ to obtain powder I;
step four: and (3) forming, namely pressing and forming the powder material I under the pressure of 30MPa, drying for 6h at 60 ℃, placing the dried product into a firing furnace, firing for 2h at 1300 ℃, reversing the mold, and cooling to obtain the ceramic product.
Example 7:
the seventh embodiment of the invention provides a ceramic tile, which consists of the following components in percentage by weight:
45% of quartz sand, 15% of kaolin, 7% of feldspar, 2% of talc, 2% of zircon, 2% of magnesite and 3% of spodumene.
In this embodiment, a process for preparing a ceramic tile is provided, which includes the following steps:
the method comprises the following steps: feeding and grinding, namely adding the weighed quartz sand, kaolin, feldspar, talc, zircon, magnesite and spodumene into a ball mill for grinding for 12 hours, wherein the ratio of raw materials, grinding balls and water is 1: 0.8, and preparing slurry I after grinding is finished;
step two: sieving and ageing, namely sieving the first slurry to remove iron, putting the first slurry into a slurry tank, and ageing for 10 hours to obtain first mixed slurry after ageing is finished;
step three: spray drying, namely spray drying the mixed slurry I at the hot air temperature of 500 ℃ to obtain powder I;
step four: and (3) forming, namely pressing and forming the powder material I under the pressure of 30MPa, drying for 6h at 60 ℃, placing the dried product into a firing furnace, firing for 2h at 1300 ℃, reversing the mold, and cooling to obtain the ceramic product.
Example 8:
the eighth embodiment of the invention provides a ceramic tile, which consists of the following components in percentage by weight:
45% of quartz sand, 15% of kaolin, 7% of feldspar, 1% of talc, 3% of zircon, 2% of magnesite and 2% of spodumene.
In this embodiment, a process for preparing a ceramic tile is provided, which includes the following steps:
the method comprises the following steps: feeding and grinding, namely adding the weighed quartz sand, kaolin, feldspar, talc, zircon, magnesite and spodumene into a ball mill for grinding for 12 hours, wherein the ratio of raw materials, grinding balls and water is 1: 0.8, and preparing slurry I after grinding is finished;
step two: sieving and ageing, namely sieving the first slurry to remove iron, putting the first slurry into a slurry tank, and ageing for 10 hours to obtain first mixed slurry after ageing is finished;
step three: spray drying, namely spray drying the mixed slurry I at the hot air temperature of 500 ℃ to obtain powder I;
step four: and (3) forming, namely pressing and forming the powder material I under the pressure of 30MPa, drying for 6h at 60 ℃, placing the dried product into a firing furnace, firing for 2h at 1300 ℃, reversing the mold, and cooling to obtain the ceramic product.
Table one: formulation table (unit: kg) of composite antibacterial ceramic tile in each embodiment
Examples 1 to 4 are composite antibacterial ceramic tiles prepared according to the present invention, and examples 5 to 8 are antibacterial ceramic tiles prepared by a conventional process.
Specifically, the composite antibacterial ceramic tiles prepared in examples 1 to 8 and the commercially available antibacterial ceramic tiles were subjected to comparative tests. In addition, 50 parts of each of the composite antibacterial ceramic tiles prepared in examples 1 to 8 and commercially available antibacterial ceramic tiles were subjected to performance comparison tests, and the corresponding test results are shown in table two.
Table two: results of performance tests on the composite antibacterial ceramic tiles manufactured in examples 1 to 8 and comparative commercially available antibacterial ceramic tiles
As can be seen from the above table:
compared with the antibacterial ceramic tile prepared by the traditional process, the composite antibacterial ceramic tile prepared by the preparation method has longer-acting antibacterial ability than the ceramic tile prepared by the traditional process.
In the above embodiments, since the tile strength is greatly affected by the ratio of carbon nitride to graphene, the tile fire resistance is greatly affected by the ratio of magnesite to zircon, the tile antibacterial property is greatly affected by the ratio of copper nitrate, silver nitrate and bentonite, and the tile glaze glossiness is greatly affected by the ratio of wollastonite, talc and nepheline. Therefore, comprehensive comparison shows that the composite antibacterial ceramic tile manufactured by the formula in the third embodiment has the optimal performance.
The invention has the beneficial effects that: the composite antibacterial ceramic tile manufactured by the invention has the advantages of simple process, easily obtained raw materials, safety and no toxicity. Meanwhile, the composite antibacterial ceramic tile has high strength, good fire resistance, good sterilization effect, long sterilization duration and good glaze glossiness in the use process.
The specific process of the invention is as follows:
preparing bentonite and silver nitrate according to the formula amount, and preparing a nano silver-loaded inorganic antibacterial agent taking the bentonite as a carrier by adopting an ion exchange method for later use;
taking kaolin, feldspar, quartz sand, zircon, magnesite, spodumene and copper nitrate according to the formula ratio, uniformly mixing the raw materials, adding the raw materials into a ball mill, grinding for 8-10 h, wherein the ratio of the raw materials to grinding balls to water is 1: 0.8: 0.5, sieving by a 100-150-mesh sieve after grinding, carrying out spray drying after sieving, removing most of nitric acid in the copper nitrate in the spray drying process at the hot air temperature of 450-500 ℃, and collecting dried powder to obtain mixed powder I;
crushing nepheline, talc and wollastonite according to the formula, sieving the crushed nepheline, talc and wollastonite with a 200-300-mesh sieve, adding the crushed nepheline, talc and wollastonite and the mixed powder I into a stirrer, adding sodium silicate with solid content of 35 percent and weight of 3-7 percent of the mixture, stirring and mixing for 20min, adding a nano silver-loaded inorganic antibacterial agent with bentonite as a carrier, stirring for 20-30 min again, pressing and molding powder under the pressure of 30-40MPa after stirring, and drying for 3-4 h at the temperature of 60-70 ℃ to obtain a dry blank;
raising the temperature of the prepared dry blank to 850-900 ℃ at a heating rate of 10-15 ℃/min, preserving heat for 1-2 h, decomposing copper oxide by the copper removed by nitric acid at high temperature, raising the temperature to 1200-1300 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 3-4 h, melting and releasing the copper oxide to the surface of the blank at the raising temperature due to the low melting point of nepheline, driving part of the copper oxide and the nano silver-loaded inorganic antibacterial agent taking bentonite as a carrier to move outwards, reducing the temperature to 340-380 ℃ at a cooling rate of 6-8 ℃/min, preserving heat for 2-3 h, cooling to normal temperature, edging, and packaging to obtain the finished product.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The composite antibacterial ceramic tile is characterized by comprising the following components in percentage by weight: 20-45% of quartz sand, 15-20% of kaolin, 5-7% of feldspar, 5-7% of copper nitrate, 8-10% of wollastonite, 1-2% of talc, 5-7% of nepheline, 5-8% of an antibacterial agent, 6-9% of auxiliary materials and 5-10% of reinforcing materials, wherein the auxiliary materials comprise zircon, magnesite and spodumene, the antibacterial agent comprises bentonite and silver nitrate, and the reinforcing materials comprise carbon nitride and graphene.
2. The composite antibacterial ceramic tile according to claim 1, wherein the auxiliary materials comprise the following components in percentage by weight:
zircon 2% -3%, magnesite 2% -3% and spodumene 2% -3%.
3. The composite antibacterial ceramic tile according to claim 2, wherein the antibacterial agent comprises the following components in percentage by weight:
3 to 5 percent of bentonite and 2 to 3 percent of silver nitrate.
4. The composite antibacterial ceramic tile according to claim 3, wherein the reinforcing material comprises the following components in percentage by weight:
2 to 6 percent of carbon nitride and 3 to 4 percent of graphene.
5. The composite antibacterial ceramic tile according to claim 4, characterized in that the composite antibacterial ceramic tile comprises the following components by weight percent:
35% of quartz sand, 15% of kaolin, 5% of feldspar, 5% of copper nitrate, 10% of wollastonite, 1% of talc, 5% of nepheline, 3% of zircon, 3% of magnesite, 3% of spodumene, 3% of bentonite, 2% of silver nitrate, 6% of carbon nitride and 4% of graphene.
6. The composite antibacterial ceramic tile according to claim 4, characterized in that the composite antibacterial ceramic tile comprises the following components by weight percent:
30% of quartz sand, 20% of kaolin, 5% of feldspar, 7% of copper nitrate, 10% of wollastonite, 1% of talc, 5% of nepheline, 3% of zircon, 3% of magnesite, 3% of spodumene, 5% of bentonite, 3% of silver nitrate, 2% of carbon nitride and 3% of graphene.
7. The composite antibacterial ceramic tile according to claim 4, characterized in that the composite antibacterial ceramic tile comprises the following components by weight percent:
20% of quartz sand, 20% of kaolin, 7% of feldspar, 7% of copper nitrate, 10% of wollastonite, 2% of talc, 7% of nepheline, 3% of zircon, 3% of magnesite, 3% of spodumene, 5% of bentonite, 3% of silver nitrate, 6% of carbon nitride and 4% of graphene.
8. A process for the preparation of composite antibacterial ceramic tiles, characterized in that it is used for the preparation of composite antibacterial ceramic tiles according to any one of the preceding claims 1 to 7, said process comprising the following steps:
the method comprises the following steps: preparing bentonite and silver nitrate according to the formula amount, and preparing a nano silver-loaded inorganic antibacterial agent taking the bentonite as a carrier by adopting an ion exchange method for later use;
step two: taking kaolin, feldspar, quartz sand, zircon, magnesite, spodumene and copper nitrate according to the formula ratio, uniformly mixing the raw materials, and adding the mixture into a ball mill for grinding for 8-10 hours; wherein the ratio of the added raw materials, the grinding balls and water is 1: 0.8: 0.5, the mixture is sieved by a 100-150-mesh sieve after grinding is finished, spray drying is carried out at the hot air temperature of 450-500 ℃ after sieving, most of nitric acid in copper nitrate is removed in the spray drying process, and the mixed powder I is obtained by drying and collecting powder;
step three: crushing nepheline, talc and wollastonite according to the formula amount, sieving the crushed nepheline, talc and wollastonite with a 200-300-mesh sieve, adding the crushed nepheline, talc and wollastonite and the mixed powder I into a stirrer, adding sodium silicate with the solid content of 35 percent, which is 3-7 percent of the weight of the mixture, stirring and mixing for 20min, adding a nano silver-loaded inorganic antibacterial agent with bentonite as a carrier, carbon nitride and graphene, stirring for 20-30 min again, pressing and molding powder under the pressure of 30-40MPa after stirring, and drying for 3-4 h at the temperature of 60-70 ℃ to prepare a dry blank;
step four: raising the temperature of the prepared dry blank to 850-900 ℃ at a heating rate of 10-15 ℃/min, preserving heat for 1-2 h, decomposing copper removed by nitric acid into copper oxide at high temperature, raising the temperature to 1200-1300 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 3-4 h, melting and releasing the copper oxide to the surface of the blank at the raising temperature due to the low melting point of nepheline, driving part of the copper oxide and the nano silver-loaded inorganic antibacterial agent taking bentonite as a carrier to move outwards, reducing the temperature to 340-380 ℃ at a cooling rate of 6-8 ℃/min, preserving heat for 2-3 h, cooling to normal temperature, edging, and packaging to obtain the finished product.
9. The process for preparing composite antibacterial ceramic tile according to claim 8, wherein the reaction is carried out by ion exchange method under the conditions of 120 ℃ temperature, pH less than 7 and 24h reaction time.
10. The process for preparing composite antibacterial ceramic tile according to claim 8, wherein the dry blank is printed after the preparation of the dry blank.
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