CN114195480A - Fine stain-resistant antibacterial brick and preparation method thereof - Google Patents
Fine stain-resistant antibacterial brick and preparation method thereof Download PDFInfo
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- CN114195480A CN114195480A CN202111592336.8A CN202111592336A CN114195480A CN 114195480 A CN114195480 A CN 114195480A CN 202111592336 A CN202111592336 A CN 202111592336A CN 114195480 A CN114195480 A CN 114195480A
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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- 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
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- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract
The invention discloses a fine stain-resistant antibacterial brick and a preparation method thereof. The antibacterial brick sequentially comprises a blank body, a bottom glaze layer, a high-temperature matte glaze layer, a printing layer and an antibacterial glaze layer from bottom to top; the glaze slip of the antibacterial glaze layer is formed by mixing an antibacterial agent and skin glaze slip; the antibacterial agent consists of a complex of nano zinc oxide and silver iodide. The antibacterial brick has obvious antibacterial effect and can meet the antibacterial requirement of consumers; the brick surface has fine hand feeling and is effective in antifouling; the application of the antibacterial glaze enables the combination of ink-jet color development and a glaze body to be better, the texture is softer, the matte ceramic tile obtained by firing without polishing has a soft polishing effect and high glossiness, the polished ceramic tile is obtained, and the matte ceramic tile and the polished ceramic tile have the advantages of high transparency, good color development and fine and smooth bottom finish.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a fine stain-resistant antibacterial brick and a preparation method thereof.
Background
With the increasing concern of people on health, the demand of the antibacterial ceramic tile is gradually increased. At present, the conventional technique is to obtain a ceramic tile having an antibacterial effect by adding metal ions to a glaze. However, the traditional glaze has high sintering temperature, and metal ions are easy to volatilize, so that the antibacterial effect is reduced.
At present, the bright ceramic tiles on the market have smooth hand feeling and higher glossiness, but need to be polished. The matte ceramic tile has no gloss, but the surface is rough. The production process of the ceramic tile with the matte and fine and smooth handfeel is unstable, and the surface effect is difficult to control.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a fine and smooth stain-resistant antibacterial brick.
The invention also aims to provide a preparation method of the fine stain-resistant antibacterial brick.
The purpose of the invention is realized by the following technical scheme: a fine stain-resistant antibacterial brick comprises a blank body, a ground glaze layer, a high-temperature matte glaze layer, a printing layer and an antibacterial glaze layer from bottom to top in sequence; the glaze slip of the antibacterial glaze layer is formed by mixing an antibacterial agent and skin glaze slip; the antibacterial agent consists of nano zinc oxide and silver iodide complex.
Preferably, the powder of the blank is prepared from the following components in parts by weight: 32-38 parts of porcelain sand, 40-50 parts of porcelain clay, 7.5-9 parts of limestone, 3.5-5.5 parts of wollastonite and 4-10 parts of potassium feldspar.
Preferably, the preparation of the body is as follows: mixing the components in the powder, ball-milling, spray-granulating, ageing and pressing to obtain the powder.
Preferably, the time of ball milling is 12 to 16 hours.
Preferably, the aging time is 24-48 hours.
Preferably, the glaze slip of the ground glaze layer comprises the following components in parts by weight: 80-85 parts of ground glaze frit, 4-6 parts of potassium feldspar, 6-9 parts of calcined talc, 8-13 parts of air knife soil, 0.3 part of carboxymethyl cellulose, 0.4 part of sodium tripolyphosphate, 20-30 parts of water and 4-7 parts of titanium dioxide; the ground glaze frit comprises the following components in parts by weight: 25-35 parts of potassium feldspar, 15-25 parts of calcite, 10-15 parts of dolomite, 10-15 parts of titanium dioxide, 20-30 parts of quartz sand and 2-5 parts of phosphorus calcium powder.
Preferably, the glaze slip of the ground glaze layer is prepared as follows: ball-milling the components until the fineness of glaze slurry reaches 100 meshes, sieving with 325 meshes, sieving with 100 meshes when the residue is less than 0.5%, and aging to obtain the final product; preparing the ground glaze frit: the components are mixed, calcined and melted at 1480 ℃, and water quenched to obtain the glaze slip reaching the bottom glaze layer.
Preferably, the time of ball milling is 12 to 16 hours.
Preferably, the aging time is 24-48 hours.
Preferably, the glaze slip of the high-temperature matte glaze layer comprises the following components in parts by weight: 80-85 parts of matte frit, 8-12 parts of zirconium silicate, 3-5 parts of calcined kaolin, 5-8 parts of air knife soil, 0.1-0.4 part of methyl cellulose, 0.2-0.6 part of sodium tripolyphosphate and 29% of water by weight of dry materials; the matte frit comprises the following components in parts by weight: calcite: 7-10 parts of barium carbonate, 7-14 parts of potassium feldspar, 35-45 parts of potassium feldspar, 4-10 parts of zinc oxide, 6-15 parts of calcined kaolin, 0.5-4 parts of boric acid, 1.0-1.5 parts of soda ash, 8-15 parts of quartz sand, 1-6 parts of strontium carbonate and 2-4 parts of dolomite.
Preferably, the glaze slip of the high-temperature matte glaze layer is prepared as follows: mixing the components, performing ball milling, sieving the obtained glaze slurry with a 60-100 mesh sieve, then with a 325 mesh sieve, sieving the glaze slurry with a 80-120 mesh sieve when the residue of the sieve reaches 0.1-0.6%, and aging to obtain the glaze slurry; the matte frit was prepared as follows: mixing the components, calcining and melting at 1400-1600 ℃, and water quenching.
Preferably, the time of the ball milling is 8 to 12 hours.
Preferably, the aging time is 12 to 48 hours.
The glaze slip of the antibacterial glaze layer is formed by mixing skin glaze slip and an antibacterial agent; preferably, the dosage of the antibacterial agent is 0.2-1% of the weight of the skin glaze slip; more preferably, the antibacterial agent is used in an amount of 0.2 to 0.5% by weight of the skin glaze slip.
The skin glaze slip comprises the following components in parts by weight: 80-85 parts of skin glaze frit, 10-12 parts of calcined kaolin, 5-7 parts of zinc oxide, 0.1-0.4 part of methyl cellulose, 0.2-0.6 part of sodium tripolyphosphate and 29% of water by weight of dry materials; the skin glaze frit comprises the following components in parts by weight: 8-11 parts of calcite, 7-11 parts of barium carbonate, 1-2 parts of strontium carbonate, 40-55 parts of potassium feldspar, 10-15 parts of kaolin, 2-5 parts of calcium borate, 1-2 parts of soda ash, 9-12 parts of quartz sand and 1-3 parts of dolomite.
Preferably, the skin glaze slip is prepared as follows: mixing the components, performing ball milling, sieving the obtained glaze slurry with a sieve of 80-120 meshes, then sieving with a sieve of 325 meshes, sieving the glaze slurry with a sieve of 80-120 meshes when the residue of the sieve reaches 0.1-0.6%, and aging to obtain the glaze slurry; matte frits were prepared as follows: the components are mixed, calcined and melted at 1400 ℃ and 1600 ℃, and water quenched to obtain the skin glaze slip.
Preferably, the time of the ball milling is 8 to 12 hours.
Preferably, the aging time is 12 to 48 hours.
Preferably, the antibacterial agent comprises nano zinc oxide and silver iodide complex, and the mass ratio of the nano zinc oxide to the silver iodide complex is 0.5-1.2: 0.4-2; more preferably, the mass ratio of the nano zinc oxide to the silver iodide complex is 1: 1.
preparation of the silver iodide complex: mixing the silver nitrate solution and the potassium iodide solution, standing, filtering, washing by distilled water, centrifuging and drying to obtain the silver iodide complex.
Preferably, the concentration of the potassium iodide solution is 1.1 mol/L.
Preferably, the concentration of the silver nitrate solution is 1.1-1.3 mol/L.
Preferably, the silver nitrate solution is added to a potassium iodide solution in an amount of 3% excess of potassium iodide over silver nitrate.
Preferably, the temperature of the drying is 0-60 ℃.
The preparation method of the fine stain-resistant antibacterial brick comprises the following steps: firing the blank into a biscuit, spraying base glaze slip on the biscuit, spraying high-temperature matte glaze slip, printing, spraying antibacterial glaze slip, and firing again to obtain the fine and pollution-resistant antibacterial brick.
Preferably, the firing temperature is 1100-.
Preferably, the flow rate of the bottom glaze slip is 30-45s, and the specific gravity is 1.75-1.85g/m3And the glazing amount is 300 x 600mm, and the brick spraying amount is 65-100 g/piece.
Preferably, the flow rate of the glaze slip is 30-45s, and the specific gravity is 1.75-1.95g/m3And the glazing amount is 300 x 600mm, and the brick spraying amount is 60-100 g/piece.
Preferably, the printing means may be ink-jet printing, roller, screen, or a combination thereof.
Preferably, the flow rate of the antibacterial glaze slip is 30-45s, and the specific gravity is 1.75-1.95g/m3And the glazing amount is 300 x 600mm, and the brick spraying amount is 60-100 g/piece.
Preferably, the secondary firing is carried out at 1080-1200 ℃ for 40-60 min.
Compared with the prior art, the invention has the following beneficial effects:
1. the antibacterial brick has a remarkable antibacterial effect and can meet the antibacterial requirement of consumers. Titanium dioxide is added into the ground glaze layer, and firstly, the titanium dioxide can be tightly combined with the biscuit and is not easy to run off; secondly, the titanium dioxide can generate active oxygen and hydroxyl radical with sterilization effect after absorbing ultraviolet; moreover, the absorbed ultraviolet is beneficial to the oxidation of the nano zinc oxide, the sterilization effect is improved, the sterilization is rapid and lasting, the usage amount of the antibacterial agent is small, and the production cost is reduced;
2. the brick surface of the antibacterial brick has fine hand feeling, and is effective in antibiosis and antifouling;
3. the antibacterial glaze is applied, so that the combination of ink-jet color development and a glaze body is better, the texture is softer, the matte ceramic tile obtained by firing without polishing has a soft polishing effect and high glossiness, and the bright ceramic tile is obtained after polishing; the matt ceramic tile and the bright ceramic tile have high transparency, good color development and fine and smooth bottom light.
Drawings
FIG. 1 is a photograph of the antibacterial brick prepared in example 1.
FIG. 2 is a photograph of the antibacterial brick prepared in example 2.
FIG. 3 is a photograph of the antibacterial brick prepared in example 3.
Fig. 4 is a comparison of the effects of the matte antibacterial brick and the bright antibacterial brick prepared in example 4.
FIG. 5 is a graph of the antibacterial brick and stain resistance test prepared in example 4; wherein, a is the antibacterial brick without ink, b is the antibacterial brick after ink is coated, and c is the antibacterial brick after the ink on the surface is removed by washing after 30 min.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
1. Preparation of the starting materials
The following raw materials are used in parts by weight.
a. Mixing 35 parts of porcelain sand, 45 parts of porcelain clay, 8 parts of limestone, 4 parts of wollastonite and 8 parts of potassium feldspar, putting the mixture into a ball mill, carrying out wet ball milling for 12 hours, carrying out spray granulation, and carrying out ageing for 24 hours to obtain blank powder, and pressing the blank powder by using a press to obtain a blank.
b. Mixing 80 parts of ground glaze frit, 6 parts of potassium feldspar, 7 parts of burning talc, 8 parts of air knife soil (Hengfeng company), 25 parts of water, 0.3 part of carboxymethyl cellulose, 0.4 part of sodium tripolyphosphate and 5 parts of titanium dioxide, putting the mixture into a ball mill, carrying out ball milling for 15 hours until the fineness of the glaze slurry reaches 100 meshes, then sieving the glaze slurry by 325 meshes, sieving the glaze slurry by 100 meshes when the screen residue is less than 0.5%, and ageing the glaze slurry for 25 hours to obtain the ground glaze slurry.
Wherein the ground glaze frit: 35 parts of potassium feldspar, 20 parts of calcite, 10 parts of dolomite, 10 parts of titanium dioxide, 22 parts of quartz sand and 3 parts of phosphorus-calcium powder: the components are mixed, calcined and melted at 1480 ℃, and water quenched to obtain the ground glaze frit.
c. Mixing 80 parts of matte frit, 9 parts of zirconium silicate, 5 parts of calcined kaolin, 6 parts of air knife soil (Hengfeng company), 0.3 part of methyl cellulose, 0.4 part of sodium tripolyphosphate and 29% of water by weight of dry materials, putting the mixture into a ball mill, carrying out ball milling for 13 hours to obtain glaze slurry, firstly sieving the glaze slurry with a 80-mesh sieve, then sieving the glaze slurry with a 325-mesh sieve, sieving the glaze slurry with a 100-mesh sieve when the surplus of the sieve reaches 0.4%, and carrying out ageing for 25 hours to obtain the high-temperature matte glaze slurry.
Wherein, the matte frit: calcite: 10 parts, 12 parts of barium carbonate, 43 parts of potassium feldspar, 5 parts of zinc oxide, 8 parts of calcined kaolin, 3 parts of boric acid, 1 part of soda ash, 14 parts of quartz sand, 2 parts of strontium carbonate and 2 parts of dolomite. The components are mixed, calcined and melted at 1500 ℃, and water quenched to obtain the matte frit.
d. Mixing 85 parts of skin glaze frit, 10 parts of calcined kaolin, 5 parts of zinc oxide, 0.3 part of methyl cellulose, 0.4 part of sodium tripolyphosphate and 29% of water by weight of dry materials, adding the mixture into a ball mill, carrying out ball milling for 12 hours, sieving the obtained glaze slurry with a 90-mesh sieve and then with a 325-mesh sieve, sieving the glaze material with a 110-mesh sieve when the screen residue reaches 0.5%, and carrying out aging for 30 hours to obtain the skin glaze slurry.
Wherein, the skin glaze frit: 10 parts of calcite, 10 parts of barium carbonate, 2 parts of strontium carbonate, 45 parts of potassium feldspar, 12 parts of kaolin, 2 parts of soda ash, 10 parts of quartz sand and 2 parts of dolomite; mixing the above raw materials, adding into a frit furnace, calcining at 1500 deg.C for melting, flowing out of the frit furnace, and water quenching to obtain skin glaze frit.
e. And d, adding three thousandths of antibacterial agent (nano zinc oxide and silver iodide complex with the mass ratio of 1: 1) into the skin glaze slip obtained in the step d, and performing ball milling for 10 minutes to obtain the antibacterial skin glaze slip.
Preparing a silver iodide complex; stirring potassium iodide solution with concentration of 1.1mol/L, simultaneously adding silver nitrate solution with concentration of 1.2mol/L until the mass of potassium iodide is more than 3% of that of potassium iodide, generating yellow silver iodide precipitate, standing, filtering, washing with distilled water, centrifuging, and drying at 55 deg.C.
2. Preparation of antibacterial brick
a. Firing the blank body into a biscuit at 1200 ℃, spraying base glaze slurry through a bell jar glaze sprayer, and uniformly distributing the glaze slurry on the blank body, wherein the glaze spraying parameters are as follows: the flow rate of the glaze slip is 30s, and the specific gravity is 1.75g/m3Glazing amount of 300 x 600mm/70 g/piece;
b. spraying high-temperature matte glaze slip through a bell jar glaze sprayer, and uniformly spraying glaze on a blank body coated with the ground glaze slip, wherein the parameters are as follows: the flow rate of the glaze slip is 40s, and the specific gravity is 1.8g/cm3The glaze amount is 300 × 600mm, and 60 g/piece of brick is sprayed;
c. performing ink-jet printing on the blank body coated with the high-temperature matte glaze slip;
d. uniformly spreading the antibacterial skin glaze slip on the surface of the blank after ink-jet printing through a bell jar glaze sprayer, wherein the flow rate of the glaze slip is 40s, and the specific gravity is 1.75g/m3The glaze amount is 300 x 600mm/75 g/piece;
e. and (3) placing the ceramic tile blank body coated with the antibacterial skin glaze slip into a roller kiln for high-temperature firing at 1100 ℃ for 45 minutes, and performing subsequent edge grinding and grading to obtain the antibacterial brick shown in the figure 1.
As can be seen from FIG. 1, the antibacterial brick is fine and smooth, high in glossiness, high in transparency and good in color development.
Example 2
1. Preparation of the starting materials
The following raw materials are used in parts by weight.
a. Mixing 35 parts of porcelain sand, 45 parts of porcelain clay, 8 parts of limestone, 4 parts of wollastonite and 8 parts of potassium feldspar, putting the mixture into a ball mill, carrying out wet ball milling for 12 hours, carrying out spray granulation, and carrying out ageing for 24 hours to obtain blank powder, and pressing the blank powder by using a press to obtain a blank.
b. Mixing 80 parts of ground glaze frit, 6 parts of potassium feldspar, 7 parts of burning talc, 7 parts of air knife soil (Hengfeng company), 0.3 part of carboxymethyl cellulose, 0.4 part of sodium tripolyphosphate, 5 parts of titanium dioxide and 25 parts of water, putting the mixture into a ball mill, performing ball milling for 12 hours until the fineness of the glaze slurry reaches 100 meshes, then performing 325 meshes, performing 100 meshes when the screen residue is less than 0.5%, and performing ageing for 28 hours to obtain the ground glaze slurry. The composition and preparation of the ground glaze frit were the same as in example 1.
c. 85 parts of matte frit, 10 parts of zirconium silicate, 4 parts of calcined kaolin, 5 parts of air-knife soil, 0.3 part of methyl cellulose, 0.3 part of sodium tripolyphosphate and 29% of water by weight of dry materials are added into a ball mill, the obtained glaze slurry is sieved by a 70-mesh sieve and then by a 325-mesh sieve, when the screen residue reaches 0.2%, the glaze is sieved by a 80-mesh sieve and is aged for 35 hours, and the high-temperature matte glaze slurry is obtained. The matte frit composition and preparation were the same as in example 1.
d. Mixing 85 parts of skin glaze frit, 10 parts of calcined kaolin, 5 parts of zinc oxide, 0.1-0.4 part of methyl cellulose, 0.2-0.6 part of sodium tripolyphosphate and 29% of water by weight of dry materials, adding the mixture into a ball mill, carrying out ball milling for 16 hours, sieving the obtained glaze slurry with a sieve of 80-120 meshes firstly, then sieving with a sieve of 325 meshes, sieving the glaze material with a sieve of 80-120 meshes when the screen residue reaches 0.1-0.6%, and carrying out ageing for 15 hours to obtain the skin glaze slurry. The formulation of the skin glaze frit was the same as in example 1.
e. And d, adding three thousandth of antibacterial agent (nano zinc oxide and silver iodide complex with the mass ratio of 0.5: 1) into the skin glaze slip obtained in the step d, and performing ball milling for ten minutes to obtain the antibacterial skin glaze slip. The silver iodide complex was prepared as in example 1.
2. Preparation of antibacterial brick
a. Firing the blank body into a biscuit at 1200 ℃, spraying base glaze slurry through a bell jar glaze sprayer, and uniformly distributing the glaze slurry on the blank body, wherein the glaze spraying parameters are as follows: glaze slipThe flow rate is 35s, and the specific gravity is 1.85g/cm3And the glaze amount is 300 x 600mm, and the brick spraying amount is 70 g/piece.
b. Uniformly applying high-temperature matte glaze slip on the blank body on which the base glaze slip is applied by a bell jar glaze spraying device, wherein the glaze spraying parameters are as follows: the flow rate of the glaze slip is 40s, and the specific gravity is 1.8g/cm3And the glaze amount is 300 x 600mm, and the brick is poured by 100 g/piece.
c. And performing ink-jet printing on the blank body coated with the high-temperature matte glaze slip.
d. Uniformly applying the antibacterial skin glaze slip on the surface of the blank after ink-jet printing through a bell jar glaze sprayer, wherein the flow rate of the glaze slip is 45s, and the specific gravity is 1.9g/m3The glaze amount is 300 x 600mm/85 g/piece.
e. And (3) placing the ceramic tile blank body coated with the antibacterial skin glaze slip into a roller kiln, firing at a high temperature of 1110 ℃ for 46 minutes, and performing subsequent processing, edge grinding and grading to obtain the antibacterial brick shown in the figure 2. It can be seen that the antibacterial brick is fine and smooth, high in glossiness, high in transparency and good in color development.
Example 3
1. Preparation of the starting materials
a. Mixing 35 parts of porcelain sand, 45 parts of porcelain clay, 8 parts of limestone, 4 parts of wollastonite and 8 parts of potassium feldspar, putting the mixture into a ball mill, carrying out wet ball milling for 12 hours, carrying out spray granulation, and carrying out ageing for 24 hours to obtain blank powder, and pressing the blank powder by using a press to obtain a blank.
b. Mixing 80 parts of ground glaze frit, 6 parts of potassium feldspar, 7 parts of burning talc, 8 parts of air knife soil (Hengfeng company), 0.3 part of carboxymethyl cellulose, 0.4 part of sodium tripolyphosphate, 20 parts of water and 6 parts of titanium dioxide, putting the mixture into a ball mill, performing ball milling for 13 hours until the fineness of the glaze slurry reaches 100 meshes, then performing 325 meshes, performing 100 meshes when the screen residue is less than 0.5%, and performing ageing for 40 hours to obtain the ground glaze slurry. The formulation and preparation of the ground glaze frit were the same as in example 1.
c. Mixing 80 parts of matte frit, 9 parts of zirconium silicate, 5 parts of calcined kaolin, 6 parts of air knife soil (Hengfeng company), 0.1 part of methyl cellulose, 0.5 part of sodium tripolyphosphate and 29% of water by weight of dry materials, putting the mixture into a ball mill, carrying out ball milling for 16 hours to obtain glaze slurry, firstly sieving the glaze slurry with a 100-mesh sieve, then sieving the glaze slurry with a 325-mesh sieve, sieving the glaze slurry with an 80-mesh sieve when the surplus of the sieve reaches 0.6%, and carrying out ageing for 15 hours to obtain the high-temperature matte glaze slurry. The formulation and preparation of the high temperature matte glaze frit were the same as in example 1.
d. Mixing 85 parts of skin glaze frit, 10 parts of calcined kaolin, 5 parts of zinc oxide, 0.1 part of methyl cellulose, 0.4 part of sodium tripolyphosphate and 29% of water by weight of dry materials, adding the mixture into a ball mill, carrying out ball milling for 15 hours, sieving the obtained glaze slurry with a 90-mesh sieve, then sieving the glaze slurry with a 325-mesh sieve, sieving the glaze slurry with a 110-mesh sieve when the screen residue reaches 0.2%, and carrying out aging for 30 hours to obtain the skin glaze slurry. The formulation and preparation of the skin glaze frit were the same as in example 1.
e. And d, adding five thousandths of antibacterial agent (nano zinc oxide and silver iodide complex compound with the mass ratio of 1.2: 0.8) into the skin glaze slip obtained in the step d, and performing ball milling for ten minutes to obtain the antibacterial skin glaze slip. The silver iodide complex was prepared as in example 1.
2. Preparation of antibacterial brick
a. Firing the blank body at 1100 ℃ to obtain a biscuit, spraying the ground glaze slip through a bell jar glaze sprayer, and uniformly distributing the glaze slip on the blank body, wherein the spraying parameters are that the flow rate of the ground glaze slip is 30s, and the specific gravity is 1.75g/cm3And 300 x 600mm brick spraying 70 g/piece.
b. Pouring high-temperature matte glaze slip through a bell jar glaze pouring device, and uniformly pouring glaze on a blank body on which the ground glaze slip is spread, wherein the glaze pouring parameters are as follows: the flow rate of the glaze slip is 35s, and the specific gravity is 1.85g/cm3300 x 600mm brick shower 65 g/piece.
c. And performing ink-jet printing on the blank body coated with the high-temperature matte glaze slip.
d. Uniformly distributing the antibacterial skin glaze slip on the surface of the blank after ink-jet printing through a bell jar glaze spraying device, wherein the glaze spraying parameters are as follows: the flow rate of the glaze slip is 40s, and the specific gravity is 1.8g/cm3The glaze amount is 300 x 600mm, and 65 g/piece of glaze is poured in each piece.
e. And (3) placing the ceramic tile blank body coated with the antibacterial skin glaze slip into a roller kiln for high-temperature firing at 1120 ℃ for 45 minutes, and performing subsequent processing, edge grinding, grading and polishing to obtain the antibacterial brick shown in the figure 3. It can be seen that the antibacterial brick is fine and smooth, high in transparency and good in color development.
Example 4
1. Preparation of the starting materials
a. Mixing 35 parts of porcelain sand, 45 parts of porcelain clay, 8 parts of limestone, 4 parts of wollastonite and 8 parts of potassium feldspar, putting the mixture into a ball mill, carrying out wet ball milling for 12 hours, carrying out spray granulation, and carrying out ageing for 24 hours to obtain blank powder, and pressing the blank powder by using a press to obtain a blank.
b. Mixing 80 parts of ground glaze frit, 6 parts of potassium feldspar, 7 parts of calcined talc, 12 parts of air knife soil (Hengfeng company), 0.3 part of carboxymethyl cellulose, 0.4 part of sodium tripolyphosphate, 20 parts of water and 6 parts of titanium dioxide, putting the mixture into a ball mill, carrying out ball milling for 13 hours until the fineness of the glaze slurry reaches 100 meshes, then sieving the glaze slurry by 325 meshes, sieving the glaze slurry by 100 meshes when the screen residue is less than 0.5%, and carrying out ageing for 45 hours to obtain the ground glaze slurry. The formulation and preparation of the ground glaze frit were the same as in example 1.
c. 80 parts of matte frit, 9 parts of zirconium silicate, 5 parts of calcined kaolin, 6 parts of air knife soil (Hengfeng company), 0.2 part of methyl cellulose, 0.6 part of sodium tripolyphosphate and 29% of water by weight of dry materials are mixed and put into a ball mill for ball milling for 16 hours, the obtained glaze slurry is firstly sieved by a 70-mesh sieve and then sieved by a 325-mesh sieve, when the surplus of the sieve reaches 0.1%, the glaze is sieved by a 100-mesh sieve and is aged for 15 hours, and the high-temperature matte glaze slurry is obtained. The formulation and preparation of the matte frit were the same as in example 1.
d. Mixing 85 parts of skin glaze frit, 10 parts of calcined kaolin, 5 parts of zinc oxide, 0.3 part of methyl cellulose, 0.2 part of sodium tripolyphosphate and 29% of water by weight of dry materials, adding the mixture into a ball mill, carrying out ball milling for 16 hours, sieving the obtained glaze slurry with a 90-mesh sieve, then sieving the glaze slurry with a 325-mesh sieve, sieving the glaze slurry with a 90-mesh sieve when the surplus of the glaze reaches 0.3%, and carrying out ageing for 45 hours to obtain the skin glaze slurry. The formulation and preparation of the skin glaze frit were the same as in example 1.
e. And d, adding two weight percent of antibacterial agent (nano zinc oxide and silver iodide complex with the mass ratio of 0.8: 1.6) into the skin glaze slip obtained in the step d, and performing ball milling for ten minutes to obtain the antibacterial skin glaze slip. The silver iodide complex was prepared as in example 1.
2. Preparation of antibacterial brick
a. Firing the blank body into a biscuit at 1200 ℃, spraying base glaze slip through a bell jar glaze sprayer, and uniformly distributing the base glaze slip on the blank body, wherein the spraying parameters are as follows: the flow rate of the glaze slip is 35s, and the specific gravity is 1.75g/cm3And 300 x 600mm bricks are sprayed for 60 g/piece.
b. Spraying high-temperature matte glaze slip through a bell jar glaze sprayer, and uniformly spraying glaze on a blank body coated with the ground glaze slip, wherein the parameters are as follows: the flow rate of the glaze slip is 40s, and the specific gravity is 1.95g/cm3300 x 600mm brick shower 65 g/piece.
c. And (4) performing ink-jet printing on the brick surface coated with the high-temperature matte glaze slip. The functional ink with the engraving and milling function can be added according to different products.
d. Uniformly distributing the antibacterial skin glaze slip on the surface of the blank after ink-jet printing through a bell jar glaze sprayer, wherein the parameters are as follows: the flow rate of the glaze slip is 40s, and the specific gravity is 1.8g/m3The glaze amount is 300 × 600mm showers 65 g/piece.
e. And (3) placing the ceramic tile blank obtained in the step (5) into a roller kiln for high-temperature firing at 1120 ℃ for 46 minutes, performing subsequent processing, edging and grading to obtain a matte antibacterial brick, and polishing to obtain a bright antibacterial brick, wherein the comparison of the effects of the matte antibacterial brick and the bright antibacterial brick is shown in FIG. 4. As can be seen, the matte antibacterial brick is not polished, but has soft polishing effect and high glossiness; both the two kinds of ceramic tiles have fine and smooth hand feeling, high transparency and good color development.
Comparative examples 1 to 2
The comparative examples 1 and 2 are different from example 1 in that the antibacterial agents used are nano zinc oxide and silver iodide, respectively, and the dosage of the antibacterial agents is two percent of the weight of the skin glaze slip.
Comparative examples 3 to 6
Comparative examples 3 to 6 are different from example 1 in that the mass ratio of nano zinc oxide to silver iodide in the nano zinc oxide and silver iodide complex is 2: 1. 3: 1. 1: 2. 1: 3.
performance detection
1. The antibacterial bricks of examples 1-4 (figures 1-4) and comparative examples 1-6 are respectively taken to test the surface wear resistance, stain resistance and static friction coefficient according to the methods specified in GB/T3810-2006 and GB/T4100-2006, and the results are all qualified. The stain resistance test of example 4 is shown in fig. 5, the ink is coated on the antibacterial brick, and the antibacterial brick is washed after 30min to check whether the ink is left on the brick surface.
2. The antibacterial bricks of examples 1-4 and comparative examples 1-6 are respectively tested for antibacterial performance by a JC/T897-2014 test method, and antibacterial durability by a GB/T9266 test method, and the results are shown in Table 1.
The results show that the antibacterial bricks of examples 1-4 have good antibacterial performance and antibacterial durability, and are obviously higher than the national standard. The antibacterial bricks of comparative examples 1 and 2 are samples prepared by the same method and five batches, the antibacterial rates of the samples are respectively 40% -80% and 50% -90%, and are not only obviously lower than those of examples 1-4, but also the antibacterial rates of different samples are different greatly, the antibacterial effect is unstable, and the antibacterial durability is poor. The antibacterial bricks of comparative examples 3 to 6 were not as effective as those of the antibacterial bricks of the examples of the present invention.
TABLE 1
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. The fine stain-resistant antibacterial brick is characterized by comprising a blank body, a ground glaze layer, a high-temperature matte glaze layer, a printing layer and an antibacterial glaze layer from bottom to top in sequence; the glaze slip of the antibacterial glaze layer is formed by mixing an antibacterial agent and skin glaze slip; the antibacterial agent comprises nano zinc oxide and silver iodide complex.
2. The fine stain-resistant antibacterial brick according to claim 1, wherein the antibacterial agent is used in an amount of 0.2-1% by weight of the skin glaze slip; the mass ratio of the nano zinc oxide to the silver iodide complex is 0.5-1.2: 0.4-2.
3. The fine stain-resistant antibacterial brick according to claim 2, wherein the antibacterial agent is used in an amount of 0.2-0.5% by weight of the skin glaze slip; the mass ratio of the nano zinc oxide to the silver iodide complex is 1: 1.
4. the antibacterial tile of claim 1, wherein the silver iodide complex is prepared by: mixing the silver nitrate solution and the potassium iodide solution, standing, filtering, washing by distilled water, centrifuging and drying to obtain the silver iodide complex.
5. The fine stain resistant antibacterial brick according to claim 4,
the concentration of the potassium iodide solution is 1.1 mol/L;
the concentration of the silver nitrate solution is 1.1-1.3 mol/L;
adding a potassium iodide solution into the silver nitrate solution, wherein the using amount of the potassium iodide solution is that the potassium iodide is 3% more than that of the silver nitrate;
the drying temperature is 0-60 ℃.
6. The fine stain resistant antibacterial brick according to claim 1,
the skin glaze slip comprises the following components in parts by weight: 80-85 parts of skin glaze frit, 10-12 parts of calcined kaolin, 5-7 parts of zinc oxide, 0.1-0.4 part of methyl cellulose, 0.2-0.6 part of sodium tripolyphosphate and 29% of water by weight of dry materials; the skin glaze frit comprises the following components in parts by weight: 8-11 parts of calcite, 7-11 parts of barium carbonate, 1-2 parts of strontium carbonate, 40-55 parts of potassium feldspar, 10-15 parts of kaolin, 2-5 parts of calcium borate, 1-2 parts of soda ash, 9-12 parts of quartz sand and 1-3 parts of dolomite;
the glaze slip of the ground glaze layer comprises the following components in parts by weight: 80-85 parts of ground glaze frit, 4-6 parts of potassium feldspar, 6-9 parts of calcined talc, 8-13 parts of air knife soil, 0.3 part of carboxymethyl cellulose, 0.4 part of sodium tripolyphosphate, 20-30 parts of water and 4-7 parts of titanium dioxide; the ground glaze frit comprises the following components in parts by weight: 25-35 parts of potassium feldspar, 15-25 parts of calcite, 10-15 parts of dolomite, 10-15 parts of titanium dioxide, 20-30 parts of quartz sand and 2-5 parts of phosphorus calcium powder.
7. The fine stain resistant antibacterial brick according to claim 6,
the skin glaze slip is prepared as follows: mixing the components, performing ball milling, sieving the obtained glaze slurry with a sieve of 80-120 meshes, then sieving with a sieve of 325 meshes, sieving the glaze slurry with a sieve of 80-120 meshes when the residue of the sieve reaches 0.1-0.6%, and aging to obtain the glaze slurry; the matte frit was prepared as follows: mixing the components, calcining and melting at 1400-1600 ℃, and water quenching to obtain skin glaze slip;
the glaze slip of the ground glaze layer is prepared as follows: ball-milling the components until the fineness of glaze slurry reaches 100 meshes, sieving with 325 meshes, sieving with 100 meshes when the residue is less than 0.5%, and aging for 24-48 hours to obtain the final product; preparing the ground glaze frit: the components are mixed, calcined and melted at 1480 ℃, and water quenched to obtain the glaze slip reaching the bottom glaze layer.
8. The fine stain resistant antibacterial brick according to claim 1,
the powder of the blank is prepared from the following components in parts by weight: 32-38 parts of porcelain sand, 40-50 parts of porcelain clay, 7.5-9 parts of limestone, 3.5-5.5 parts of wollastonite and 4-10 parts of potassium feldspar;
the glaze slip of the high-temperature matte glaze layer comprises the following components in parts by weight: 80-85 parts of matte frit, 8-12 parts of zirconium silicate, 3-5 parts of calcined kaolin, 5-8 parts of air knife soil, 0.1-0.4 part of methyl cellulose, 0.2-0.6 part of sodium tripolyphosphate and 29% of water by weight of dry materials; the matte frit comprises the following components in parts by weight: calcite: 7-10 parts of barium carbonate, 7-14 parts of potassium feldspar, 35-45 parts of potassium feldspar, 4-10 parts of zinc oxide, 6-15 parts of calcined kaolin, 0.5-4 parts of boric acid, 1.0-1.5 parts of soda ash, 8-15 parts of quartz sand, 1-6 parts of strontium carbonate and 2-4 parts of dolomite.
9. The method for preparing the fine stain-resistant antibacterial brick according to any one of claims 1 to 8, characterized by comprising the following steps: and firing the blank body at 1100-.
10. The method for preparing the fine stain-resistant antibacterial brick according to claim 9, wherein,
the flow rate of the glaze slip is 30-45s, and the specific gravity is 1.75-1.85g/m3The glaze amount is 300 x 600mm, and the brick spraying amount is 65-100 g/piece;
the flow rate of the glaze slip is 30-45s, and the specific gravity is 1.75-1.95g/m3The glaze amount is 300 x 600mm, and the brick is sprayed by 60-100 g/piece;
the flow rate of the glaze slip is 30-45s, and the specific gravity is 1.75-1.95g/m3And the glaze amount is 300 x 600mm, and the brick spraying amount is 60-100 g/piece.
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