CN111730729B - Preparation method of antibacterial and bacteriostatic glazed tile and preparation method of nano antibacterial liquid thereof - Google Patents
Preparation method of antibacterial and bacteriostatic glazed tile and preparation method of nano antibacterial liquid thereof Download PDFInfo
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- CN111730729B CN111730729B CN202010764471.5A CN202010764471A CN111730729B CN 111730729 B CN111730729 B CN 111730729B CN 202010764471 A CN202010764471 A CN 202010764471A CN 111730729 B CN111730729 B CN 111730729B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/08—Apparatus or processes for treating or working the shaped or preshaped articles for reshaping the surface, e.g. smoothing, roughening, corrugating, making screw-threads
- B28B11/0845—Apparatus or processes for treating or working the shaped or preshaped articles for reshaping the surface, e.g. smoothing, roughening, corrugating, making screw-threads for smoothing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
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- 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
- C03C2204/00—Glasses, glazes or enamels with special properties
- C03C2204/02—Antibacterial glass, glaze or enamel
Abstract
The invention discloses a preparation method of an antibacterial glazed tile and a preparation method of a nano antibacterial liquid thereof, which comprises the following specific steps: s1) keeping the baked, discharged, cooled and cooled glazed tile within a specified temperature range at a constant temperature, and carrying out polishing and antifouling treatment on the glazed tile, wherein the glaze of the glazed tile contains an antibacterial agent; s2) dripping nano antibacterial super-clean A-type polishing solution on the surface of a glaze layer of the glazed tile, and polishing and waxing the glazed tile by adopting a pressed millstone, wherein the antibacterial A-type polishing solution comprises nano antibacterial solution and super-clean A-type polishing solution, and the super-clean A-type polishing solution is super-clean polishing solution containing silicon resin; s3) polishing and waxing are qualified, and the antibacterial glazed tile is prepared. The preparation method of the nano antibacterial liquid provided by the invention is simple and effective in process, and the prepared antibacterial glazed tile has a good antibacterial effect and stable and lasting antibacterial performance.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a preparation method of an antibacterial glazed brick and a preparation method of a nano antibacterial liquid thereof.
Background
Ceramic glazed tiles are the most widely used decorative building materials and frequently contact with human beings. The traditional glazed tile has many micro-nano level pits and gaps on the glaze surface, and provides hiding and breeding places for bacteria.
The antibacterial agent in the glaze layer of the antibacterial glazed tile has a contact antibacterial action mechanism, in the production process of the glazed tile, the glaze usually needs to be added with super-clean polishing solution for polishing, the glaze is added with a coating of the super-clean polishing solution, and the coating of the super-clean polishing solution does not contain antibacterial substances, so that after the antibacterial agent in the glaze layer is covered by the coating of the super-clean polishing solution, part of the antibacterial agent is wrapped by the coating, and the proportion of the antibacterial agent in the glaze layer which can be in contact with bacteria is reduced, so that the antibacterial performance of the antibacterial glazed tile is reduced.
Disclosure of Invention
The invention provides a preparation method of an antibacterial and bacteriostatic glazed tile and a preparation method of a nano antibacterial liquid thereof. The invention also provides a preparation method of the nano antibacterial liquid, and the preparation method is simple and effective.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an antibacterial glazed tile comprises the following specific steps:
s1) placing the baked, discharged, cooled and cooled glazed tile in a constant temperature environment within a specified temperature range, and polishing and cleaning the glazed tile, wherein the glaze of the glazed tile contains an antibacterial agent;
s2) in the same constant temperature environment as that in the step S1, an antibacterial A-type polishing solution is dripped on the surface of the glaze layer of the glazed tile, a pressurized millstone is adopted to polish and wax the glazed tile, the antibacterial A-type polishing solution comprises a nano antibacterial solution and an ultra-clean and bright A-type polishing solution, and the ultra-clean and bright A-type polishing solution is an ultra-clean and bright polishing solution containing silicon resin;
s3) polishing and waxing are qualified, and the antibacterial glazed tile is prepared.
Preferably, the following steps are further included between step S2 and step S3:
s2.1) in the same constant temperature environment as that in the step S1, dropwise adding an antibacterial D-type polishing solution on the surface of a glaze layer of the glazed tile, polishing and waxing the glazed tile by adopting a pressing millstone, wherein the antibacterial D-type polishing solution comprises a nano antibacterial solution and an ultra-clean and bright D-type polishing solution, and the ultra-clean and bright D-type polishing solution contains silicone oil.
Preferably, the temperature range specified in the step S1 is 60 to 75 ℃, and the pressure applied by the grinding disc in the step S2 is 0.1 to 0.5 MPa.
Preferably, in step S2, when the pH of the ultra-clean and bright type a polishing solution is 5 to 7, the nano antibacterial solution comprises the following raw material components in parts by weight: 2-10 parts of phosphoric acid or oxalic acid, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of a mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1; when the pH value of the ultra-clean and bright A-type polishing solution is 8-10, the nano antibacterial solution comprises the following raw materials in parts by weight: 0.5-1.5 parts of defoaming agent, 30-50 parts of triethanolamine, 10-50 parts of polyquaternium 126, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1.
Preferably, the antibacterial A-type polishing solution and the antibacterial D-type polishing solution both contain 2-10% of the nano antibacterial liquid by mass percent; the dropping amount of the antibacterial A-type polishing solution and the antibacterial D-type polishing solution in the steps S2 and S2.1 is 10-20g/m2。
Preferably, the antibacterial A-type polishing solution and the antibacterial D-type polishing solution both contain 3-6% of the nano antibacterial liquid by mass percent.
Preferably, the glaze of step S1 contains the antibacterial agent which is a mixture of silver-loaded nano-zirconium silicate and nano-zinc oxide, and the silver-loaded nano-zirconium silicate is added in an amount of 0.2-2% of the total weight of the glaze of the glazed tile, and the nano-zinc oxide is added in an amount of 0.1-1% of the total weight of the glaze of the glazed tile, calculated by weight percentage.
Preferably, the mixing ratio of the silver-loaded nano-zirconium silicate to the nano-zinc oxide is 2:1, and the particle size of the silver-loaded nano-zirconium silicate to the nano-zinc oxide is 10-15 nm.
Further, the invention also provides a preparation method of the nano antibacterial liquid, and the preparation method of the antibacterial and bacteriostatic glazed tile by using the nano antibacterial liquid comprises the following specific steps:
p1), when the pH value of the ultra-clean and bright A-type polishing solution is 5-7, the nano antibacterial solution comprises the following raw materials in parts by weight: 2-10 parts of phosphoric acid or oxalic acid, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of a mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1; when the pH value of the ultra-clean and bright A-type polishing solution is 8-10, the nano antibacterial solution comprises the following raw materials in parts by weight: 0.5-1.5 parts of defoaming agent, 30-50 parts of triethanolamine, 10-50 parts of polyquaternium 126, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1;
p2) adding the mixture of the nano antibacterial liquid into the water slurry, and putting the mixture into a ball mill for ball milling to obtain the nano antibacterial liquid.
Further, the rotation speed of the ball mill in the step P2 is 60-120 r/min, and the ball milling time is 1 hour.
The invention has the beneficial effects that:
according to the preparation method of the antibacterial and bacteriostatic glazed tile, the glaze layer of the prepared antibacterial and bacteriostatic glazed tile contains the antibacterial agent, and the antibacterial material is added into polishing solution for polishing and waxing, so that the polished coating also has the antibacterial and bacteriostatic functions, and the defect that the antibacterial effect is reduced after the conventional polished coating of the antibacterial glazed tile is used for a period of time is overcome.
Even if the polishing and waxing coating is worn after the antibacterial and bacteriostatic glazed tile is used for a period of time, the antibacterial performance of the glaze layer of the antibacterial and bacteriostatic glazed tile still exists, and the durability of the antibacterial effect of the antibacterial and bacteriostatic glazed tile can be improved.
The invention also provides a simple and effective preparation method of the antibacterial liquid.
Detailed Description
The technical solution of the present invention is further described below in specific embodiments.
A preparation method of an antibacterial glazed tile comprises the following specific steps:
s1) placing the baked, discharged, cooled and cooled glazed tile in a constant temperature environment within a specified temperature range, and polishing and cleaning the glazed tile, wherein the glaze of the glazed tile contains an antibacterial agent;
s2) in the same constant temperature environment as that in the step S1, an antibacterial A-type polishing solution is dripped on the surface of the glaze layer of the glazed tile, a pressurized millstone is adopted to polish and wax the glazed tile, the antibacterial A-type polishing solution comprises a nano antibacterial solution and an ultra-clean and bright A-type polishing solution, and the ultra-clean and bright A-type polishing solution is an ultra-clean and bright polishing solution containing silicon resin;
s3) polishing and waxing are qualified, and the antibacterial glazed tile is prepared.
The antibacterial mechanism of the nano silver oxide and the nano zinc oxide in the glaze layer of the antibacterial glazed tile is mainly contact antibacterial, in the production process of the glazed tile, the glaze usually needs to be added with ultra-clean polishing solution for polishing, and the antibacterial performance of the antibacterial glazed tile is reduced due to the addition of the coating of the ultra-clean polishing solution.
According to the preparation method of the antibacterial and bacteriostatic glazed tile, disclosed by the invention, the antibacterial material is added into the polishing solution for polishing and waxing, so that the polished coating has an antibacterial and bacteriostatic function, and even if the polished and waxed coating is worn after the antibacterial and bacteriostatic glazed tile is used for a period of time, the antibacterial performance of the glaze layer of the antibacterial and bacteriostatic glazed tile still exists, and the durability of the antibacterial effect of the antibacterial and bacteriostatic glazed tile can be improved.
Preferably, the following steps are further included between step S2 and step S3:
s2.1) in the same constant temperature environment as that in the step S1, dropwise adding an antibacterial D-type polishing solution on the surface of a glaze layer of the glazed tile, polishing and waxing the glazed tile by adopting a pressing millstone, wherein the antibacterial D-type polishing solution comprises a nano antibacterial solution and an ultra-clean and bright D-type polishing solution, and the ultra-clean and bright D-type polishing solution contains silicone oil.
The ultra-clean and bright A-type polishing solution and the ultra-clean and bright D-type polishing solution used in the invention are commercially available ultra-clean and bright polishing solutions, the ultra-clean and bright D-type polishing solution contains silicone oil components and can play an antifouling role, and the ultra-clean and bright A-type polishing solution contains silicone resin components and mainly serves to fill micro pores of a glaze surface.
Through the first adoption the polishing of super bright A type polishing solution is waxed, the reuse contains the silicon oil composition super bright D type polishing solution carries out the polishing of second and is waxed, can further improve antibiotic antibacterial glazed tile's antifouling performance and antibiotic efficiency, contain through twice polishing the addition super bright D type polishing solution with the coating of super bright A type polishing solution can have tighter protection, has better antibiotic bacteriostasis.
Preferably, the temperature range specified in the step S1 is 60 to 75 ℃, and the pressure applied by the grinding disc in the step S2 is 0.1 to 0.5 MPa.
Has the advantages that: the surface temperature of the glazed tile is in the range of 60-75 ℃ during waxing, which is beneficial to the solidification of ultra-clean and bright silicone resin, the removal of redundant moisture during polishing, and the solidification and uniform distribution of the nano antibacterial liquid in pores on the surface.
Preferably, in step S2, when the pH of the ultra-clean and bright type a polishing solution is 5 to 7, the nano antibacterial solution comprises the following raw material components in parts by weight: 2-10 parts of phosphoric acid or oxalic acid, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of a mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1; when the pH value of the ultra-clean and bright A-type polishing solution is 8-10, the nano antibacterial solution comprises the following raw materials in parts by weight: 0.5-1.5 parts of defoaming agent, 30-50 parts of triethanolamine, 10-50 parts of polyquaternium 126, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1.
According to the super-bright polishing solution, if the acid-base system balance of the super-bright A-type polishing solution is broken due to overlarge acid-base change, the super-bright A-type polishing solution can be condensed into gel, so that the super-bright A-type polishing solution cannot be used, the pH value of the raw material component of the added nano antibacterial solution needs to be adjusted to be close to the pH value of the super-bright A-type polishing solution according to the pH value of the super-bright A-type polishing solution, and the mixed solution of the nano antibacterial solution and the super-bright A-type polishing solution with the adjusted formula has better antifouling and antibacterial effects.
The triethanolamine and the polyquaternium 126 are pH value regulators of the nano antibacterial liquid under the alkaline condition, and the triethanolamine is also a good chelating agent which is beneficial to the dispersion and the stability of the nano zinc oxide and the nano silver oxide; the polyquaternium 126 also has an antibacterial function and is beneficial to enhancing the antibacterial performance of the nano antibacterial liquid.
And the phosphoric acid or oxalic acid is used for adjusting the pH value of the nano antibacterial liquid under an acidic condition.
The dispersing agent is sodium polyacrylate and sodium tripolyphosphate, and the mixed solution of the nano antibacterial solution and the ultra-clean and bright A-type polishing solution can obtain a uniform dispersing effect by only adding a small amount of the dispersing agent.
The silane coupling agent is simultaneously linked with the silicon resin of the ultra-clean and bright A-type polishing solution, and the inorganic antibacterial agent nano silver oxide and nano zinc oxide, so that the whole antibacterial system is more stable.
The antifoaming agent mainly has the effects of reducing the viscosity of the antibacterial liquid under an alkaline condition and avoiding the influence of too many bubbles on the distribution of the antibacterial liquid, and the adopted trademark is Tween 80 or Tween 100.
Zn contained in nano zinc oxide and nano silver oxide2+Or Ag+Can directly act with bacteria because of Zn2+Or Ag+Can destroy the activity of active enzyme of bacterial cell membrane or cell protoplasm at very low concentration, damage the three-dimensional structure (denaturation), and cause dysfunction in a short time, so that Zn2+Or Ag+Is toxic to microorganisms (bacteria, molds, viruses also broadly include algae and protozoa), strongly attracts enzyme proteins in bacteria, rapidly binds to the enzyme which is an essential group, inactivates the enzyme, and causes the bacteria to die, and when the bacteria are killed, Zn is added2+Or Ag+And the water can be dissociated out of the water tank,and the bacterial colonies are contacted with other bacterial colonies to play a new round of antibacterial action, and the process is repeated.
Preferably, the antibacterial A-type polishing solution and the antibacterial D-type polishing solution both contain 2-10% of the nano antibacterial liquid by mass percent; the dropping amount of the antibacterial A-type polishing solution and the antibacterial D-type polishing solution in the steps S2 and S2.1 is 10-20g/m2。
The dropping amount of the antibacterial D-type polishing solution is less than 10g/m2The ceramic tile has insufficient luster and poor antifouling performance due to too little polishing solution, and has little influence on the antibacterial performance, and the dropping amount of the antibacterial D-type polishing solution is more than 20g/m2Too much results in the surface of the tile being difficult to dry, having a greasy feel and affecting the use feel of the user.
Preferably, the antibacterial A-type polishing solution and the antibacterial D-type polishing solution both contain 3-6% of the nano antibacterial liquid by mass percent.
The antibacterial A-type polishing solution and the antibacterial D-type polishing solution contain 3-6% of the nano antibacterial liquid by mass percent, and have a better antibacterial effect.
Preferably, the glaze of step S1 contains the antibacterial agent which is a mixture of silver-loaded nano-zirconium silicate and nano-zinc oxide, and the silver-loaded nano-zirconium silicate is added in an amount of 0.2-2% of the total weight of the glaze of the glazed tile, and the nano-zinc oxide is added in an amount of 0.1-1% of the total weight of the glaze of the glazed tile, calculated by weight percentage.
Under the condition that no antibacterial material is added into the polishing solution, the addition amount of an antibacterial agent of a glaze layer of the existing antibacterial glazed tile is higher, the addition amount of the silver-loaded nano zirconium silicate is 2-6% of the total weight of the glaze of the glazed tile, and the addition amount of the nano zinc oxide is 1-3% of the total weight of the glaze of the glazed tile.
After the antibacterial material is added into polishing solution for polishing, the polishing and waxing coating has an antibacterial effect, under the condition that the glaze layer and the coating simultaneously play an antibacterial role, the addition of the antibacterial agent of the glaze layer can be reduced on the premise of ensuring the integral antibacterial effect, the addition of the silver-carrying nano zirconium silicate is reduced to 0.2-2% from 2-6% of the total weight of glaze of the glazed tile, and the addition of the nano zinc oxide is reduced to 0.1-1% from 1-3% of the total weight of the glaze of the glazed tile, so that a good antibacterial effect can be obtained, the integral cost can be reduced, and the cost performance of the prepared antibacterial and bacteriostatic glazed tile can be improved.
Preferably, the mixing ratio of the silver-loaded nano-zirconium silicate to the nano-zinc oxide is 2:1, and the particle size of the silver-loaded nano-zirconium silicate to the nano-zinc oxide is 10-15 nm.
Theoretically, the smaller the particle size of the nano silver oxide and the nano zinc oxide, the better the antibacterial activity is, but the smaller the particle size is, the production cost is high, the agglomeration is easy to cause the reduction of the antibacterial performance, the particle size of 10-15 nm in the prior art is easy to realize, and the antibacterial effect is better.
Further, the invention also provides a preparation method of the nano antibacterial liquid, and the preparation method of the antibacterial and bacteriostatic glazed tile by using the nano antibacterial liquid comprises the following specific steps:
p1), when the pH value of the ultra-clean and bright A-type polishing solution is 5-7, the nano antibacterial solution comprises the following raw materials in parts by weight: 2-10 parts of phosphoric acid or oxalic acid, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of a mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1; when the pH value of the ultra-clean and bright A-type polishing solution is 8-10, the nano antibacterial solution comprises the following raw materials in parts by weight: 0.5-1.5 parts of defoaming agent, 30-50 parts of triethanolamine, 10-50 parts of polyquaternium 126, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1;
p2) adding the mixture of the nano antibacterial liquid into the water slurry, and putting the mixture into a ball mill for ball milling to obtain the nano antibacterial liquid.
The preparation method is simple and effective, and the main purpose of ball milling is to uniformly disperse various components of the nano antibacterial liquid and to add a proper amount of water to homogenize the slurry.
Further, the rotation speed of the ball mill in the step P2 is 60-120 r/min, and the ball milling time is 1 hour.
The ball milling speed is controlled to be 60-120 r/min, and the effect of uniform dispersion can be achieved after the ball milling time is 1 hour.
Examples 1 to 12
The antibacterial and bacteriostatic glazed tile of each example was prepared as follows:
1. the preparation method of the antibacterial and bacteriostatic glazed tile in each embodiment comprises the following specific steps:
s1) placing the baked, discharged, cooled and cooled glazed tile in a constant temperature environment within a specified temperature range, and polishing and cleaning the glazed tile, wherein the glaze of the glazed tile contains an antibacterial agent;
s2) in the same constant temperature environment as that in the step S1, nanometer antibacterial super-bright A-type polishing solution is dripped on the surface of the glaze layer of the glazed tile, a pressurized millstone is adopted to polish and wax the glazed tile, the antibacterial A-type polishing solution comprises nanometer antibacterial liquid and super-bright A-type polishing solution, and the super-bright A-type polishing solution is super-bright polishing solution containing silicon resin;
s2.1) dripping nano antibacterial super-bright D-type polishing solution on the surface of the glaze layer of the glazed tile in the same constant temperature environment as the step S1, and polishing and waxing the glazed tile by adopting a pressed millstone, wherein the antibacterial D-type polishing solution comprises nano antibacterial liquid and super-bright D-type polishing solution, and the super-bright D-type polishing solution is super-bright polishing solution containing silicone oil;
s3) polishing and waxing are qualified, and the antibacterial glazed tile is prepared.
The temperature range specified in the step S1 is 60-75 ℃, and the pressure applied by the grinding disc in the step S2 is 0.1-0.5 MPa;
the antibacterial A-type polishing solution and the antibacterial D-type polishing solution both contain 2-10% of the nano antibacterial liquid by mass percent; the dripping amount of the antibacterial A-type polishing solution or the antibacterial D-type polishing solution in the steps S2 and S2.1 is 10-20g/m2；
The glaze of step S1 contains the antibacterial agent which is a mixture of silver-loaded nano-zirconium silicate and nano-zinc oxide, and calculated according to the weight percentage, the addition amount of silver-loaded nano-zirconium silicate is 0.2-2% of the total weight of the glaze of the glazed tile, the addition amount of nano-zinc oxide is 0.1% -1% of the total weight of the glaze of the glazed tile, the mixing ratio of silver-loaded nano-zirconium silicate and nano-zinc oxide is 2:1, the particle size of silver-loaded nano-zirconium silicate and nano-zinc oxide is 10-15 nm, and the content of silver-loaded nano-zirconium silicate and nano-zinc oxide specifically added in examples 1-12 is shown in table 1.
2. The preparation method of the nano antibacterial liquid of the preparation method of the antibacterial and bacteriostatic glazed tile in each embodiment comprises the following specific steps:
p1), when the pH value of the ultra-clean and bright A-type polishing solution is 5-7, the nano antibacterial solution comprises the following raw materials in parts by weight: 2-10 parts of phosphoric acid or oxalic acid, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of a mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1; when the pH value of the ultra-clean and bright A-type polishing solution is 8-10, the nano antibacterial solution comprises the following raw materials in parts by weight: 0.5-1.5 parts of defoaming agent, 30-50 parts of triethanolamine, 10-50 parts of polyquaternium 126, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1;
p2) adding water into the mixture of the nano antibacterial liquid, and putting the mixture into a ball mill for ball milling to obtain the nano antibacterial liquid;
the rotating speed of the ball mill in the step P2 is 60-120 r/m, and the ball milling time is 1 hour.
When the pH value of the ultra-clean and bright A-type polishing solution of the embodiments 1 to 6 is 5 to 7, the nano antibacterial solution comprises the following raw material components in parts by weight: 2-10 parts of phosphoric acid or oxalic acid, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of a mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2:1, wherein the components and the proportion of the specifically added raw materials of examples 1-6 are shown in Table 1;
when the pH value of the ultra-clean and bright A-type polishing solution of embodiments 7 to 12 is 8 to 10, the nano antibacterial solution comprises the following raw material components in parts by weight: 0.5-1.5 parts of defoaming agent, 30-50 parts of triethanolamine, 10-50 parts of polyquaternium 126, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of a mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2:1, wherein the trademark of the defoaming agent is Tween 80, and the components and the proportion of the specifically added raw materials in examples 7-12 are shown in Table 1;
4. the antibacterial and bacteriostatic glazed tiles prepared in examples 1-12 are sampled according to JC/T897-2014 (antibacterial performance of antibacterial ceramic products), and the relevant antibacterial rate and antibacterial durability are detected, wherein the detection results of the examples are shown in Table 1.
Comparative examples 1 to 10
1. The glazed tile of comparative example 1 contained the same amount of the antibacterial agent as in example 2, and was not subjected to any polishing and waxing treatment;
2. the glazed tile of comparative example 2 contains the same antibacterial agent content as in example 2, and the polishing and waxing treatment is carried out according to the same procedure as the preparation method of the antibacterial and bacteriostatic glazed tile of example 2, except that: the polishing solution used in the step S2 is ultra-clean and bright A-type polishing solution, the polishing solution used in the step S2.1 is ultra-clean and bright D-type polishing solution, and the nano antibacterial solution is not added;
3. the difference between the preparation method of the antibacterial and bacteriostatic glaze of the comparative example 3 and the example 2 is that: the step of the preparation method of the antibacterial and bacteriostatic glazed tile of the comparative example 3 does not contain S2;
4. the differences between the preparation methods of the antibacterial and bacteriostatic glaze surfaces of the comparative examples 4 and 5 and the example 2 are as follows: the components of the nano antibacterial liquid added in the comparative examples 4 and 5 are different, and the details are shown in table 2;
5. comparative examples 6 and 7 differ from example 2 in that: the nano antibacterial liquid mixed with the ultra-clean and bright A-type polishing liquid contains different silane coupling agent contents;
6. comparative examples 8, 9 and 10 differ from example 2 in that: the constant temperature range values in the polishing and waxing process are different, and are shown in table 2 specifically;
7. according to the JC/T897-2014 antibacterial performance of antibacterial ceramic products, the antibacterial and bacteriostatic glazed tiles prepared in the comparative examples 1-10 are sampled and the related antibacterial rate and antibacterial durability performance are detected, and the detection results of each proportion are shown in the table 2.
TABLE 1 data and information on and test results of the examples
The following is an analysis explanation based on the above cases and test results of the respective examples and comparative examples:
1. according to the standard requirement of JC/T897-2014 antibacterial ceramic product antibacterial performance, the antibacterial rate (%) of the antibacterial performance is more than or equal to 90 percent and the antibacterial rate (%) of the antibacterial durability is more than or equal to 85 percent.
2. The pH values of examples 1 to 6 are between 5 and 7, the pH values of examples 7 to 12 are between 8 and 10, the antibacterial rates (%) of the antibacterial performance and the antibacterial durability of the examples 1 to 12 are all more than 90%, and the antibacterial rates (%) of the antibacterial durability are all more than 85%, and all the results are qualified; the polishing and waxing of the embodiment 1 does not contain the step S2.1, and the detection result is qualified, but the antibacterial rate of the antibacterial performance and the antibacterial rate of the antibacterial durability performance of the polishing and waxing are lower than the numerical values of the embodiment 2-12; the nano antibacterial liquid added in the steps S2 and S2.1 has more effective antibacterial and bacteriostatic effects in the polishing and waxing process;
the glaze of examples 1 to 12 contains the antibacterial agent which is a mixture of silver-loaded nano-zirconium silicate and nano-zinc oxide, and calculated by weight percentage, the addition amount of silver-loaded nano-zirconium silicate is 0.2 to 2% of the total weight of the glaze of the glazed tile, the addition amount of nano-zinc oxide is 0.1 to 1% of the total weight of the glaze of the glazed tile, the mixing ratio of silver-loaded nano-zirconium silicate to nano-zinc oxide is 2:1, the particle size of silver-loaded nano-zirconium silicate and nano-zinc oxide is 10 to 15 nanometers, and the antibacterial and bacteriostatic glazed tile still has a good antibacterial and bacteriostatic effect, which indicates that the preparation method of the antibacterial and bacteriostatic glazed tile has a significant beneficial effect;
when the pH value of the ultra-clean and bright A-type polishing solution of the embodiments 1 to 6 is 5 to 7, the nano antibacterial solution comprises the following raw material components in parts by weight: 2-10 parts of phosphoric acid or oxalic acid, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of a mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1;
when the pH value of the ultra-clean and bright A-type polishing solution of embodiments 7 to 12 is 8 to 10, the nano antibacterial solution comprises the following raw material components in parts by weight: 0.5-1.5 parts of defoaming agent, 30-50 parts of triethanolamine, 10-50 parts of polyquaternium 126, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2:1, wherein the trademark of the defoaming agent is tween 80;
the antibacterial and bacteriostatic glazed tiles of the embodiments 1 to 12 have obvious antibacterial and bacteriostatic effects, which shows that good effects can be obtained by mixing the nano antibacterial liquid with different raw material components according to whether the pH value of the ultra-clean and bright A-type polishing liquid is 5 to 7 or 8 to 10.
3. Comparative examples 1-2 were analyzed, comparing to example 6:
the glazed tile of comparative example 1 contained the same amount of the antibacterial agent as in example 6, which was higher than the amount of the antibacterial agent contained in examples 1 to 5, and comparative example 1 did not undergo any polishing and waxing treatment; the detection results of the antibacterial performance and the antibacterial durability of the comparative example 1 are both qualified;
the glazed tile of comparative example 2 contains the same antibacterial agent content as in example 6, and the polishing and waxing treatment is performed according to the same procedure as the preparation method of the antibacterial and bacteriostatic glazed tile of example 6, except that: the polishing solution used in the step S2 is ultra-clean and bright A-type polishing solution, the polishing solution used in the step S2.1 is ultra-clean and bright D-type polishing solution, the nano antibacterial liquid is not added, the antibacterial rate of the antibacterial performance of the comparative example 2 is unqualified, but the detection result of the antibacterial durability performance is qualified; the method shows that the antibacterial rate of the antibacterial performance of the glazed tile which is not waxed and has qualified antibacterial performance is obviously reduced after the glazed tile is polished and waxed by the ultra-clean polishing solution; after the coating formed by polishing and waxing is damaged by washing or rubbing for many times, the antibacterial durability of the glazed tile with qualified antibacterial performance is recovered, and a good effect is still achieved;
comparing the detection result of the embodiment 2 with that of the comparative examples 1 and 2, it can be found that the adverse effects of the ultra-clean and bright A-type polishing solution or the ultra-clean and bright D-type polishing solution can be overcome by polishing and waxing the antibacterial A-type polishing solution and the antibacterial D-type polishing solution added with the nano antibacterial liquid, and the antibacterial performance and the antibacterial durability of the prepared antibacterial and bacteriostatic glazed tile can be improved, and the effect is very obvious.
4. Comparative example 3 differs from example 2 in that: the step of the preparation method of the antibacterial and bacteriostatic glazed tile of the comparative example 3 does not contain S2; the detection results of the antibacterial performance and the antibacterial durability of the antibacterial and bacteriostatic glazed tile prepared in the comparative example 3 are not qualified, which indicates that the antibacterial performance and the antibacterial durability of the antibacterial and bacteriostatic glazed tile are not improved enough only by the antibacterial liquid added in the polishing and waxing of the step S2.1, and the qualified standard cannot be met.
5. Comparative example 4 differs from example 2 in that: comparative example 4, the amount of the added nano silver oxide and nano zinc oxide is too small and is lower than the lower limit of the required standard range value, the antibacterial ability of the prepared polishing and waxing coating of the antibacterial and bacteriostatic glazed tile is too low, so that the detection results of the antibacterial performance and the antibacterial durability of the prepared antibacterial and bacteriostatic glazed tile are not qualified, and therefore, the amount of the added nano silver oxide and nano zinc oxide of the antibacterial component of the ultra-clean and bright polishing solution is controlled to be more than 10 parts.
9. Comparative example 5 differs from example 2 in that: the amount of the added nano silver oxide and the added nano zinc oxide of the antibacterial component in the comparative example 5 is too much and higher than the upper limit of the required standard range value, the antibacterial capability of the prepared polishing and waxing coating of the antibacterial and bacteriostatic glazed tile is excessive, the detection results of the antibacterial performance and the antibacterial durability of the prepared antibacterial and bacteriostatic glazed tile are qualified but are not much different from those of the example 2, and therefore, the added nano silver oxide and the added nano zinc oxide of the antibacterial component in the super-clean and bright polishing solution are controlled within 40 parts.
10. Comparative example 6 differs from example 2 in that: the silane coupling agent added in the comparative example 6 is too much and higher than the upper limit of the required standard range value, the antibacterial substance of the prepared polishing and waxing coating of the antibacterial and bacteriostatic glazed tile has good stability but excessive quality, the detection results of the antibacterial performance and the antibacterial durability of the prepared antibacterial and bacteriostatic glazed tile are qualified, but the difference with the embodiment 2 is not large, so that the silane coupling agent added in the ultra-clean and bright polishing solution is controlled within 40 parts.
11. Comparative example 7 differs from example 2 in that: the silane coupling agents added in the comparative example 7 are too few and are lower than the lower limit of the required standard range value, the stability of the antibacterial substance of the polishing and waxing coating of the prepared antibacterial and bacteriostatic glazed tile is not enough, the antibacterial performance of the prepared antibacterial and bacteriostatic glazed tile is qualified, but the detection result of the antibacterial durability performance is unqualified, so that the silane coupling agents added in the ultra-clean and bright polishing solution are more suitably controlled to be more than 5 parts.
12. Comparative examples 8, 9 and 10 differ from example 2 in that: the specified temperature range values of the constant temperature in the polishing and waxing process are different; the constant temperature treatment of the comparative example 8 is normal temperature, the specified temperature range value of the comparative example 9 is 45-60 ℃ below 60-75 ℃, and the moisture in the antibacterial A-type polishing solution and the antibacterial D-type polishing solution used for polishing and waxing cannot be fully volatilized, so that the antibacterial performance of the antibacterial and bacteriostatic glazed tile prepared by the comparative examples 8 and 9 is qualified, but the detection result of the antibacterial durability performance is unqualified; the temperature range value specified in the comparative example 10 is higher than 60-75 ℃ and is 75-90 ℃, and the excessive temperature causes the partial failure of the functions of the pH value buffering agent and the silane coupling agent in the antibacterial A-type polishing solution and the antibacterial D-type polishing solution used for polishing and waxing, so that the antibacterial performance of the antibacterial and bacteriostatic glazed tile prepared in the comparative example 10 is qualified, but the detection result of the antibacterial durability performance is unqualified.
In conclusion, the preparation method of the antibacterial and bacteriostatic glazed tile has good effect, and the antibacterial liquid and the prepared antibacterial and bacteriostatic glazed tile have good antibacterial effect and good durability.
The antibacterial liquid added in the step S2 or S2.1 of the preparation method of the antibacterial glazed tile can obtain better antibacterial effect, and the best effect can be obtained if the steps S1, S2 and S2.1 are included at the same time.
Through adding antibacterial material in the polishing solution of polishing waxing, can be so that the coating after the polishing has antibiotic bacteriostatic function, antibiotic bacteriostatic glazed tile even the coating of polishing waxing is worn and torn after using a period of time, antibiotic bacteriostatic glazed tile's the antibacterial property of glaze layer still exist, can improve antibiotic bacteriostatic glazed tile's antibiotic effect persistence.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (9)
1. A preparation method of an antibacterial glazed tile is characterized by comprising the following specific steps:
s1) placing the baked, discharged, cooled and cooled glazed tile in a constant temperature environment of 60-75 ℃, and polishing and cleaning the glazed tile, wherein the glaze of the glazed tile contains an antibacterial agent;
s2) in the same constant temperature environment as that in the step S1, an antibacterial A-type polishing solution is dripped on the surface of the glaze layer of the glazed tile, a pressurized millstone is adopted to polish and wax the glazed tile, the antibacterial A-type polishing solution comprises a nano antibacterial solution and an ultra-clean and bright A-type polishing solution, and the ultra-clean and bright A-type polishing solution is an ultra-clean and bright polishing solution containing silicon resin;
s3) polishing and waxing are qualified, and the antibacterial glazed tile is prepared;
in the step S2, when the pH value of the ultra-clean and bright type a polishing solution is 5 to 7, the nano antibacterial solution comprises the following raw material components in parts by weight: 2-10 parts of phosphoric acid or oxalic acid, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of a mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1; when the pH value of the ultra-clean and bright A-type polishing solution is 8-10, the nano antibacterial solution comprises the following raw materials in parts by weight: 0.5-1.5 parts of defoaming agent, 30-50 parts of triethanolamine, 10-50 parts of polyquaternium 126, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1.
2. The method for preparing an antibacterial and bacteriostatic glazed tile according to claim 1, wherein the following steps are further included between step S2 and step S3:
s2.1) in the same constant temperature environment as that in the step S1, dropwise adding an antibacterial D-type polishing solution on the surface of a glaze layer of the glazed tile, polishing and waxing the glazed tile by adopting a pressing millstone, wherein the antibacterial D-type polishing solution comprises a nano antibacterial solution and an ultra-clean and bright D-type polishing solution, and the ultra-clean and bright D-type polishing solution contains silicone oil.
3. The method for preparing an antibacterial and bacteriostatic glazed tile according to claim 2, wherein the pressure applied by the grinding disc in the step S2 is 0.1-0.5 MPa.
4. The method for preparing the antibacterial and bacteriostatic glazed tile according to claim 3, wherein the antibacterial A-type polishing solution and the antibacterial D-type polishing solution both contain 2-10% of the nano antibacterial liquid by mass percent; the dropping amount of the antibacterial A-type polishing solution and the antibacterial D-type polishing solution in the steps S2 and S2.1 is 10-20g/m2。
5. The preparation method of the antibacterial glazed tile according to claim 4, wherein the antibacterial A-type polishing solution and the antibacterial D-type polishing solution both contain 3-6% of the nano antibacterial liquid by mass.
6. The method for preparing an antibacterial and bacteriostatic glazed tile according to claim 1, wherein the glaze of step S1 contains the antibacterial agent which is a mixture of silver-loaded nano-zirconium silicate and nano-zinc oxide, and the addition amount of the silver-loaded nano-zirconium silicate is 0.2-2% of the total weight of the glaze of the glazed tile and the addition amount of the nano-zinc oxide is 0.1-1% of the total weight of the glaze of the glazed tile, calculated by weight percentage.
7. The preparation method of the antibacterial glazed tile according to claim 6, wherein the mixing ratio of the silver-loaded nano zirconium silicate to the nano zinc oxide is 2:1, and the particle size of the silver-loaded nano zirconium silicate to the nano zinc oxide is 10-15 nm.
8. A method for preparing nano antibacterial liquid, which is used for the method for preparing the antibacterial and bacteriostatic glazed tile as claimed in any one of claims 1 to 7, and comprises the following steps:
p1), when the pH value of the ultra-clean and bright A-type polishing solution is 5-7, the nano antibacterial solution comprises the following raw materials in parts by weight: 2-10 parts of phosphoric acid or oxalic acid, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of a mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1; when the pH value of the ultra-clean and bright A-type polishing solution is 8-10, the nano antibacterial solution comprises the following raw materials in parts by weight: 0.5-1.5 parts of defoaming agent, 30-50 parts of triethanolamine, 10-50 parts of polyquaternium 126, 0.1-1.5 parts of sodium polyacrylate, 0.1-3 parts of sodium tripolyphosphate, 5-40 parts of silane coupling agent and 10-40 parts of mixture of nano silver oxide and nano zinc oxide with the mixing ratio of 2: 1;
p2) adding the mixture of the nano antibacterial liquid into the water slurry, and putting the mixture into a ball mill for ball milling to obtain the nano antibacterial liquid.
9. The method for preparing nano antibacterial liquid according to claim 8, wherein the rotation speed of the ball mill in the step P2 is 60-120 rpm, and the time of the ball mill is 1 hour.
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| CN112341938A (en) * | 2020-10-26 | 2021-02-09 | 佛山市东鹏陶瓷有限公司 | Ceramic tile polishing solution containing composite antibacterial photocatalytic material and preparation process thereof |
| CN113248146B (en) * | 2021-06-03 | 2021-09-24 | 佛山欧神诺陶瓷有限公司 | Composite process antibacterial ceramic tile and preparation method thereof |
| CN113308138A (en) * | 2021-07-01 | 2021-08-27 | 佛山欧神诺陶瓷有限公司 | Antibacterial wax, antibacterial brick and preparation method thereof |
| CN113860854A (en) * | 2021-09-27 | 2021-12-31 | 蒙娜丽莎集团股份有限公司 | Ceramic plate with stable and durable antibacterial performance and preparation method thereof |
| CN113816772B (en) * | 2021-09-27 | 2022-12-02 | 清远纳福娜陶瓷有限公司 | Preparation method of cockroach-repelling ceramic tile and prepared cockroach-repelling ceramic tile |
| CN116640004A (en) * | 2023-05-08 | 2023-08-25 | 清远市简一陶瓷有限公司 | High-temperature-resistant antibacterial ceramic tile and preparation method thereof |
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