CN114230325B - Preparation method of antibacterial ceramic product - Google Patents
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
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- C03—GLASS; MINERAL OR SLAG WOOL
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- 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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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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
- C03C2204/00—Glasses, glazes or enamels with special properties
- C03C2204/02—Antibacterial glass, glaze or enamel
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Abstract
The invention discloses a preparation method of a self-sterilizing ceramic product, which comprises the following steps: 1) Preparing materials: preparing a blank and a glaze material according to a ratio; 2) Respectively carrying out ball milling on the blank and the glaze, preparing the blank into a blank body, and preparing the glaze; 3) Biscuit firing the blank at 820-1050 ℃ for 2.5-4.5 h; 4) Glazing the biscuit, firing the biscuit at 1150-1280 ℃ for 4-7 h, and cooling to obtain the ceramic product. The ceramic product has stable sterilization performance and sterilization durability sterilization efficiency, long time effectiveness, simple preparation process flow, easy operation and control and suitability for large-area industrial production and popularization and use.
Description
Technical Field
The invention relates to the field of inorganic non-metallic materials, in particular to a preparation method of an antibacterial ceramic product.
Background
With the increase of awareness of the public on bacteria and viruses and prevention, the demand of consumers on products with antibacterial function is gradually upgraded. Particularly, in recent years, the generation of viruses and bacteria such as novel coronavirus causes great harm to the health and life safety of people. People are more and more conscious of health, and daily ceramics are not exceptional as one of consumer products.
Although the daily ceramic product as an inorganic non-metallic material has the advantages of high melting point, high hardness, oxidation resistance and the like, the daily ceramic product is a porous product, and an uneven glaze surface is visible under a magnifying glass, so that the daily ceramic product is easy to stain and breed bacteria, and is difficult to clean after being stained.
The antibacterial domestic ceramic products in the current market have the defects of short antibacterial timeliness, poor antibacterial stability, poor antibacterial performance and antibacterial durability; the process is too complex, which is not beneficial to large-area popularization and use; the production cost is high and is limited.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of an antibacterial ceramic product, which adopts a special blank glaze formula after test optimization, a special blank glaze manufacturing process, a special firing method and a special silver-zinc-particle-carrying zirconium phosphate antibacterial agent which is safe to a human body. The antibacterial property of the ceramic product is stable and reaches more than 99.99 percent and the antibacterial durability of the ceramic product is stable and reaches more than 99.24 percent through the detection of a professional detection mechanism authorized by a national special institution, thereby solving the problems of insufficient antibacterial effect, short antibacterial aging, poor stability, complex production process and higher cost of the ceramic product in the prior art.
The invention adopts the following technical scheme:
a preparation method of an antibacterial ceramic product comprises the following steps:
1) Preparing materials: preparing raw materials according to the following mass percentages:
blank material: siO 2 2 58 to 70 percent of Al 2 O 3 18 to 28.5 percent of CaO, 0.1 to 1.5 percent of CaO, 0.1 to 1 percent of MgO and K 2 1.5 to 3.0 percent of O and Na 2 O is 0.5 to 2 percent; fe 2 O 3 0.1 to 1.5 percent; IL 5% -10% (IL is loss on ignition)
Glaze material: siO 2 2 60 to 70 percent of Al 2 O 3 6 to 12 percent of CaO, 4 to 14 percent of CaO, 1 to 3 percent of MgO and K 2 1 to 5 percent of O and Na 2 0.1 to 1.5 percent of O and Fe 2 O 3 0.01 to 0.1 percent of the total weight of the antibacterial agent, 0.5 to 3 percent of IL and more than or equal to 6 percent of the antibacterial agent; wherein the antibacterial agent is a zirconium phosphate silver-loaded zinc particle antibacterial agent;
2) Respectively carrying out ball milling on the blank and the glaze, preparing the blank into a blank body, and preparing the glaze;
3) Biscuit firing the blank at 820-1050 ℃ for 2.5-4.5 h;
4) And after biscuit firing, putting the blank into glaze to dip glaze, then firing the blank in an atmosphere of 1150-1280 ℃ for 4-7 h, and cooling to obtain the ceramic product.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts inorganic material as the antibacterial agent to be blended into the glaze, and the inorganic material can not react with the glaze in the firing process, thereby obviously improving the antibacterial capability of the ceramic product and providing a better choice for expanding the high-end market of the ceramic product in consumer goods.
2. The grain size of 70 percent of the antibacterial agent in the invention is controlled between 0.8 and 2 mu m, so that the antibacterial agent is dispersed more uniformly in the glaze, the agglomeration phenomenon is avoided, and the ceramic product has higher antibacterial performance and antibacterial durability.
3. The ceramic product prepared by the invention has the antibacterial property and the bactericidal rate of 99.99 percent on escherichia coli, and the antibacterial durability and the bactericidal rate of 99.24 percent on the escherichia coli; the antibacterial rate of staphylococcus antibacterial performance can reach more than 99.99%, and the antibacterial rate of staphylococcus antibacterial durability can reach 99.97%, which shows that compared with the antibacterial ceramic product on the market at present, the antibacterial ceramic product has stable antibacterial performance and antibacterial durability, and has lasting timeliness, and the ceramic product has the antibacterial function as long as the glaze is still in place, so that the stability and the durability of the antibacterial performance and the antibacterial durability are ensured.
4. The antibacterial glaze produced by the preparation method has the advantages of good brightness and flatness of the obtained glaze, softness and almost no pinholes on the glaze, simple whole process flow, easy operation and control, and suitability for large-area industrial production and popularization and use.
Detailed Description
The present invention will be further described with reference to the following examples.
1. Preparation method of antibacterial ceramic product
Example 1
1) Preparing materials: preparing raw materials according to the following mass percentages:
blank material: siO 2 2 69.77% of Al 2 O 3 18.91% of Fe 2 O 3 0.65%, caO 0.70%, mgO 0.47%, K 2 1.75% of O, 0.73% of Na2O and 7.02% of IL.
Glaze material: siO 2 2 66.49% of Al 2 O 3 8.37% of B 2 O 3 1.65%, caO 8.90%, mgO 1.68%, K 2 O is 3.04%, na 2 0.82% of O, liO 2 2.83%, baO 5.51%, P0.1%, fe 2 O 3 0.02%, 0.59% IL (IL for loss on ignition), 3% antimicrobial; wherein the antibacterial agent is zirconium phosphate silver-zinc particle antibacterial agent, the zirconium phosphate silver-zinc antibacterial agent is silver-zinc inorganic antibacterial agent with zirconium phosphate as carrier, and the chemical formula of zirconium phosphate is H 2 O 8 P 2 Zr is an inorganic antibacterial agent prepared by taking layered zirconium phosphate as a carrier, taking various metal ions such as silver, zinc and the like as antibacterial ions and various auxiliary agents.
2) Respectively carrying out ball milling on the blank and the glaze, preparing the blank into a blank body, and preparing the glaze; the glaze particle composition with the added antibacterial agent is <2 μm: and (5) sieving with a 325-mesh sieve until the residue is less than 0.5 percent.
3) Biscuit firing at 820 ℃ for 2.5h;
4) And glazing the green body after biscuit firing, firing the green body in an atmosphere at 1150 ℃ for 4h, and cooling to obtain the ceramic product.
Examples 2 to 5 ceramic articles examples 2 to 5 were prepared according to the process conditions of table 3 by the method of example 1, with the blanks and glaze prepared according to tables 1 and 2, respectively.
TABLE 1 blank proportioning table
| Examples | SiO 2 | Al 2 O 3 | Fe 2 O 3 | CaO | MgO | K 2 O | Na 2 O | IL |
| 1 | 69.77 | 18.91 | 0.65 | 0.7 | 0.47 | 1.75 | 0.73 | 7.02 |
| 2 | 66.37 | 21.11 | 0.94 | 0.71 | 0.42 | 2.49 | 1.14 | 6.82 |
| 3 | 58.71 | 28.42 | 0.28 | 1.46 | 0.30 | 2.80 | 1.35 | 6.68 |
| 4 | 70.00 | 18.2 | 0.20 | 0.60 | 0.90 | 2.50 | 1.10 | 6.50 |
| 5 | 62.4 | 22.55 | 0.21 | 2.1 | 0.80 | 2.50 | 0.96 | 8.48 |
Table 2 glaze proportioning table
Note: - -means that the component is not contained.
TABLE 3 Process parameters table
Remarking: d90 represents 90%; d20 represents 20%. D90<2 μm, D20<0.8 μm means that 90% of the particles have a particle size <2 μm and 20% of the particles have a particle size <0.8 μm.
The raw material proportion and the firing process of the comparative example are completely the same as those of the example, except that the grain fineness of the antibacterial agent in the comparative example is less than 0.8 μm, when the antibacterial agent is prepared with glaze, the antibacterial agent has obvious agglomeration phenomenon, the dispersion effect is poor, and the antibacterial effect of the ceramic product obtained after firing is poor.
2. Antibacterial effect
The antibacterial effects of examples 1-5 and comparative examples were tested and compared according to industry standard JC/T897-2014, see Table 4.
TABLE 4
In the prior art, when an antibacterial agent is added, the particle size of the antibacterial agent is usually controlled to be reduced, and the aim is to improve the uniformity of the antibacterial agent, but in the actual production, the particle size of the antibacterial agent is not smaller and better, but is too small, so that the antibacterial performance of the antibacterial agent is reduced, and from a comparative example, the particle size of 90% of the antibacterial agent in the comparative example is smaller than 0.8 μm. It can be seen by combining table 3 and table 4 that the fineness of the particles of the antibacterial agent in the comparative example has a significant effect on the antibacterial effect of the ceramic product, taking example 1 and comparative example 1 as examples, the raw material mixture ratio and the firing process of the two are completely the same, but the difference is that the fineness of the particles of the antibacterial agent in comparative example 1 is finer, 90% of the particles of the antibacterial agent are smaller than 0.8 μm, when the antibacterial agent is prepared with glaze, the antibacterial agent is found to have obvious agglomeration phenomenon and poor dispersion effect, and the antibacterial rate of the antibacterial performance and antibacterial durability of the comparative example 1 to escherichia coli and staphylococcus are far lower than those of example 1, which also proves that the fineness of the particles of the antibacterial agent can affect the final antibacterial effect. The method finds that the particle size of the antibacterial agent is controlled to be 0.8-2 mu m when the particle size of the antibacterial agent is researched, the antibacterial agent is more uniformly dispersed in the glaze, the agglomeration phenomenon is avoided, and the ceramic product has higher antibacterial performance and antibacterial durability. The antibacterial rate of the ceramic product prepared by the invention on escherichia coli can reach 99.99%, and the antibacterial rate of the escherichia coli with antibacterial durability can reach 99.24%; the antibacterial rate of staphylococcus with antibacterial property can reach more than 99.99%, and the antibacterial rate of staphylococcus with antibacterial durability can reach 99.97%, which shows that compared with the antibacterial ceramic product on the market at present, the antibacterial ceramic product has stable antibacterial rate and antibacterial durability, and has lasting timeliness.
3. Detection data comparison
Common antibacterial ceramic products on the market are selected for detection and comparison, and the table 6 shows.
TABLE 6
As can be seen by comparing the results in tables 4 and 6, the antibacterial rate of the ceramic product prepared by the method on Escherichia coli can reach 99.99%, and the antibacterial rate of the Escherichia coli on the durability can reach 99.24%; the antibacterial rate of the staphylococcus can reach more than 99.99%, and the antibacterial rate of the staphylococcus with antibacterial durability can reach 99.97%, which shows that compared with the antibacterial ceramic product on the market at present, the antibacterial ceramic product has stable antibacterial rate and antibacterial durability, has lasting timeliness, and ensures the stability and durability of the antibacterial rate and the antibacterial durability as long as the glaze is still in the antibacterial function of the ceramic product.
The antibacterial agent selected by the invention does not react with the glaze, thereby losing or weakening the antibacterial effect. The invention strictly screens the fineness of the antibacterial agent particles, ball-milling the glaze and the antibacterial agent together to ensure that the antibacterial agent is dispersed in the glaze more uniformly, and simultaneously, controlling the particle size of the antibacterial agent to be between 0.8 and 2 mu m, and easily causing agglomeration and being difficult to disperse if the particle size of the antibacterial agent is too fine (if the particle size is controlled to be less than 0.8 mu m). The antibacterial glaze material produced by the preparation method has the advantages of good brightness and flatness of the glaze surface, soft glaze surface, almost no pinholes, simple whole process flow, easy operation and control, and suitability for large-area industrial production and popularization and use.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and those skilled in the art should understand that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all that should be covered by the claims of the present invention.
Claims (4)
1. The preparation method of the antibacterial ceramic product is characterized by comprising the following steps of:
1) Preparing materials: preparing the following raw materials in percentage by mass:
blank material: siO 2 2 58 to 70 percent of Al 2 O 3 18 to 28.5 percent of CaO, 0.1 to 1.5 percent of CaO, 0.1 to 1 percent of MgO, and K 2 1.5 to 3.0 percent of O and Na 2 0.5% -2% of O; fe 2 O 3 0.1% -1.5%; IL is 5% -10%;
glaze material: siO 2 2 60 to 70 percent of Al 2 O 3 6-12 percent of CaO, 4-14 percent of CaO, 1-3 percent of MgO and K 2 1 to 5 percent of O and Na 2 0.1 to 1.5 percent of O and Fe 2 O 3 0.01-0.1 percent of the total amount of the antibacterial agent, 0.5-3 percent of IL and more than or equal to 10 percent of the amount of the antibacterial agent; wherein the antibacterial agent is a zirconium phosphate silver-loaded zinc particle antibacterial agent;
2) Respectively carrying out ball milling on the blank and the glaze, preparing the blank into a blank body, and preparing the glaze;
3) Biscuit firing the blank at the low temperature of 950-1050 ℃ for 3-4.5h;
4) After biscuit firing, glazing the blank, firing the blank at 1200-1280 ℃ for 5-7 h, and cooling to obtain the ceramic product;
the particle size of the antibacterial agent is D90<2 mu m, and D20<0.8 mu m;
the antibacterial agent contains 85-95% of zirconium phosphate, 0.3-0.8% of silver and 4.2-14.7% of zinc oxide;
in the step 4), the specific gravity of the glaze is 1.25 to 1.70g/ml, and the thickness of the glaze is 0.2 to 0.8mm.
2. The preparation method of the antibacterial ceramic product according to claim 1, wherein the glaze further comprises BaO, and the using amount of the BaO is 0% -11% of the total mass of the glaze; and also includes P 2 O 5 The usage amount of the glaze is 0-1.0% of the total mass of the glaze.
3. The method of manufacturing an antibacterial ceramic ware according to claim 1, wherein said glaze further comprises B 2 O 3 The using amount of the glaze is 0-4% of the total mass of the glaze; further comprises LiO 2 The usage amount of the glaze is 0-6% of the total mass of the glaze.
4. According to the claimsClaim 1 discloses a method for preparing the antibacterial ceramic product, wherein the glaze further comprises B 2 O 3 The usage amount of the glaze is 0% -4% of the total mass of the glaze; further comprises LiO 2 The usage amount of the glaze is 0% -6% of the total mass of the glaze; the glaze also comprises BaO, and the using amount of the BaO is 0-11% of the total mass of the glaze; and also includes P 2 O 5 The usage amount of the glaze is 0-1.0% of the total mass of the glaze.
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| CN100506756C (en) * | 2006-12-30 | 2009-07-01 | 江苏高淳陶瓷股份有限公司 | Technique for preparing antibiotic stoneware tableware |
| CN106517793B (en) * | 2016-11-16 | 2020-09-01 | 合众（佛山）化工有限公司 | Superfine self-cleaning glaze and preparation process thereof |
| CN109293395A (en) * | 2018-10-24 | 2019-02-01 | 东莞唛铂纳米科技有限公司 | A kind of manufacturing process of anti-bacteria ceramic |
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| CN113598165A (en) * | 2021-09-03 | 2021-11-05 | 惠州市铭铠防霉抗菌科技有限公司 | Zirconium phosphate silver-zinc-carrying composite antibacterial agent |
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