Preparation method of nano-silver enamel cover glaze antibacterial appliance

Abstract

The invention discloses a preparation method of a nano-silver enamel cover glaze antibacterial appliance. The method comprises the following steps: (1) pretreating an appliance base material; (2) preparing enamel slurry; the preparation method comprises the following steps: dissolving 4.6-5 parts by mass of alkyl imidazole in 45-55 parts by volume of water in terms of mass parts of g and volume parts of mL to obtain a solution A; taking 60-80 parts by volume of water, adding 1.5-2 parts by mass of CTAB, stirring at 35-45 DEG C, adding 4.5-5 parts by mass of silver nitrate, adding the solution A, adding 10-15 parts by mass of ammonia water, continuously stirring, dropwise adding 6-7 parts by mass of TEOS, continuously stirring, carrying out suction filtration, washing, drying, grinding, adding an ascorbic acid aqueous solution, stirring, carrying out suction filtration, adding 25-35 parts by volume of water, and uniformly stirring to obtain nano-silver antibacterial slurry; mixing the nano-silver antibacterial slurry and the enamel slurry to obtain antibacterial glaze; (3) spraying; and (4) sintering. In the invention, silver ions and alkyl imidazole form a complex which has an anchoring effect on silver, so that the agglomeration phenomenon is successfully overcome, and the antibacterial property is excellent.

Description

Technical Field

[0001] The invention belongs to the technical field of antibacterial device production, and specifically relates to a method for preparing a nano-silver enamel antibacterial device. Background Art

[0002] With the improvement of living standards and the enhancement of health awareness, the choice of kitchen utensils is increasingly tending to be safer, healthier and more efficient. As an innovative product in the field of kitchen utensils, nano-silver enamel glaze antibacterial utensils are gradually gaining favor among consumers due to their unique antibacterial properties and excellent cooking performance. The reason why this kind of utensil has an antibacterial effect is that silver ions can change the permeability of microbial cell membranes, resulting in the loss of many nutrients and metabolites, and ultimately cell death; silver ions can destroy the DNA molecules and some proteases of cells, resulting in cross-linking of DNA molecules, or catalyzing the formation of free radicals, causing viral protein denaturation, while inhibiting the electron donors on the DNA molecules, causing the DNA chain to break and thus leading to cell death. However, the problem currently encountered by companies in the process of preparing nano-silver enamel glaze antibacterial utensils is that silver ion slurry and enamel slurry will produce silver agglomeration after mixed calcination, resulting in unsatisfactory antibacterial effect. Summary of the invention

[0003] In order to overcome the shortcomings of the prior art, the purpose of the present invention is to provide a method for preparing a nano-silver enamel glaze antibacterial device.

[0004] To achieve the above purpose, the technical solution adopted by the present invention is as follows: A method for preparing a nano silver enamel antibacterial device, the steps are as follows: (1) Pretreatment: Degreasing the base material of the equipment, after which the surface should be free of wet oil stains and oily dirt; sandblasting after degreasing, after which the roughness should be between 2 and 3 and the surface should be free of obvious brightness and stains; (2) Preparation of antibacterial glaze: (2.1) Prepare enamel slurry according to the conventional formula of enamel glaze; (2.2) The mass parts are measured in g and the volume parts are measured in mL. The nano-silver antibacterial slurry is prepared according to the following steps: (2.2.1) Dissolve 4.6-5 parts by mass of alkyl imidazole in 45-55 parts by volume of water to obtain solution A; (2.2.2), take 60-80 parts by volume of water, add 1.5-2 parts by mass of CTAB, stir at 35-45°C for 30-40 minutes, then add 4.5-5 parts by mass of silver nitrate, then add solution A, then add 10-15 parts by mass of ammonia water, continue stirring for 1-1.5 hours, then drop 6-7 parts by mass of TEOS, continue stirring for 2-2.5 hours, filter it and wash it with water, send the filter cake to dry, grind it after drying, then add ascorbic acid aqueous solution according to the molar ratio of ascorbic acid: silver nitrate = (1.5-3): 1, stir for 0.4-0.7 hours, filter it, add 25-35 parts by volume of water to the filter cake, stir evenly, and obtain nano silver antibacterial slurry; (2.3), mixing the nano-silver antibacterial slurry and the enamel slurry to obtain an antibacterial glaze, based on the mass percentage of silver in the nano-silver antibacterial slurry to the enamel slurry being 0.8-1.2%; (3) Spraying: (3.1) Stir the antibacterial glaze thoroughly before use and keep stirring during use; (3.2) spraying antibacterial glaze on the surface of the utensil substrate obtained after the pretreatment in step (1); (4) Sintering: After the spraying in step (3) is completed, the surface is dried first, and then the semi-finished product after the surface drying is sent for sintering; after the sintering is completed (the coating thickness is required to be 140~170μM), it is allowed to cool and the nano silver enamel glaze antibacterial device is obtained.

[0005] Preferably, the antibacterial utensils include but are not limited to antibacterial kitchen utensils.

[0006] Preferably, in step (2.2.1), the alkyl imidazole is 2-methyl imidazole, 2-ethyl imidazole or 2-propyl imidazole.

[0007] Preferably, in step (1), the tool substrate is degreased by high-temperature degreasing, the degreasing temperature is 440-450° C., and the degreasing time is 9-10 min.

[0008] Preferably, in step (1), during the sandblasting process, 60-80 mesh brown corundum is used and the air pressure is controlled at 4.3-4.7 Pa.

[0009] Preferably, in step (2.1), based on the total weight percentage of 100%, the composition of the enamel glaze is 60-63% enamel powder, 4-5% clay, 2-4% iron black, and 30-32% water.

[0010] Preferably, in step (2.2.2), the concentration of the aqueous ammonia is 25-28 wt %.

[0011] Preferably, in step (3.2), the antibacterial glaze is sprayed with a spray gun, the nozzle diameter of the spray gun is 1.3-1.5 mm and is thoroughly cleaned with water or isopropyl alcohol before use. During spraying, the air pressure is controlled at 3-4.5 Pa.

[0012] Preferably, in step (4), the surface drying temperature is 140-150° C. and the time is 9-10 min.

[0013] Preferably, in step (4), the sintering temperature is 830-845°C and the sintering time is 4-5 min.

[0014] Beneficial effect: In the present invention, alkyl imidazole is added when preparing the antibacterial glaze, and the silver ions and the alkyl imidazole form a complex, which plays an anchoring role on the silver, successfully overcoming the agglomeration phenomenon after high-temperature sintering, so that the silver element can be evenly distributed on the surface of the utensil, thus having excellent antibacterial performance (the antibacterial rate reaches 99.99%). BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 : SEM image of the nano silver enamel glaze antibacterial pot obtained in Example 1. DETAILED DESCRIPTION

[0016] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention is further described below in conjunction with specific embodiments. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all the embodiments. Based on the described embodiments, all other embodiments obtained by those skilled in the art without creative work belong to the protection scope of the present invention.

[0017] Example 1

[0018] A method for preparing a nano silver enamel antibacterial pot, the steps are as follows: (1) Pretreatment: The pot embryo is degreased by high-temperature degreasing. The degreasing temperature is 450℃ and the time is 10 minutes. After the treatment, the surface is required to be free of wet oil stains and oil pollution. After degreasing, 60-mesh brown corundum sand is used and the air pressure is controlled at 4.5pa for sandblasting. After the treatment, the roughness is 2.5 and there is no obvious brightness and stains on the surface. (2) Preparation of antibacterial glaze: (2.1) Weigh 95 g of enamel powder, 7 g of clay, 5 g of iron black, and 50 g of deionized water, mix and grind for 8 h to obtain enamel slurry; (2.2) Prepare the nano silver antibacterial slurry according to the following steps: (2.2.1) Dissolve 4.6 g of 2-methylimidazole in 50 mL of deionized water to obtain solution A; (2.2.2) Take 80 mL of deionized water in a round-bottom flask, add 1.7 g of CTAB (hexadecyltrimethylammonium bromide) at an oil bath temperature of 40°C, stir for 30 min, add 4.7 g of silver nitrate, then add solution A, add 12 g of ammonia water (28 wt%), continue stirring for 1 h, then add 7 g of TEOS (tetraethyl orthosilicate) dropwise, continue stirring for 2 h, filter it and wash it with 1 L of deionized water, transfer the filter cake to a blast drying oven and dry it at 90°C for 12 h, grind it thoroughly after drying, then add ascorbic acid aqueous solution (concentration of 0.2 g / L) at a molar ratio of ascorbic acid:silver nitrate = 2:1, stir for 0.5 h, filter it, add 30 mL of deionized water to the filter cake, stir evenly, and obtain a nano-silver antibacterial slurry; (2.3), taking the mass percentage of silver in the nano-silver antibacterial slurry to the enamel slurry as 1%, mixing the nano-silver antibacterial slurry and the enamel slurry to obtain an antibacterial glaze; (3) Spraying: (3.1) Stir the antibacterial glaze thoroughly before use to avoid precipitation, and keep stirring during use; (3.2) Use a spray gun to spray the antibacterial glaze on the surface of the pot embryo obtained after the pretreatment in step (1). The nozzle diameter of the spray gun is 1.5 mm and it is thoroughly cleaned with deionized water before use. During spraying, the air pressure is controlled at 4.0 Pa; (4) Sintering: After the spraying in step (3) is completed, the surface is dried at 150°C for 10 minutes, and then the semi-finished product after the surface drying is placed in a muffle furnace for sintering. The sintering temperature is 835°C and the time is 5 minutes. After the sintering is completed (the coating thickness is 150μM), it is allowed to cool and the nano silver enamel glaze antibacterial pot is obtained.

[0019] Example 2

[0020] The difference from Example 1 is that in step (2.2.1), "2-ethylimidazole" is used instead of "2-methylimidazole"; the rest is the same as Example 1.

[0021] Example 3

[0022] The difference from Example 1 is that in step (2.2.1), "2-propylimidazole" is used instead of "2-methylimidazole"; the rest is the same as Example 1.

[0023] Comparative Example 1 The difference from Example 1 is that steps (2.2) and (2.3) are omitted. Specifically, this comparative example prepares a common enamel pot, and the preparation steps are as follows: (1) Pretreatment: The pot embryo is degreased by high-temperature degreasing. The degreasing temperature is 450℃ and the time is 10 minutes. After the treatment, the surface is required to be free of wet oil stains and oil pollution. After degreasing, 60-mesh brown corundum sand is used and the air pressure is controlled at 4.5pa for sandblasting. After the treatment, the roughness is 2.5 and there is no obvious brightness and stains on the surface. (2) Preparation of enamel slurry: Weigh 95 g of enamel powder, 7 g of clay, 5 g of iron black, and 50 g of deionized water, respectively, mix and grind for 8 h to obtain enamel slurry; (3) Spraying: (3.1) The enamel slurry should be fully stirred before use to avoid precipitation, and the enamel slurry should be stirred during use; (3.2) Use a spray gun to spray the enamel slurry on the surface of the pot embryo obtained after the pretreatment in step (1). The nozzle diameter of the spray gun is 1.5 mm and it is thoroughly cleaned with deionized water before use. During spraying, the air pressure is controlled at 4.0 Pa; (4) Sintering: After the spraying in step (3) is completed, the surface is dried at 150°C for 10 minutes, and then the semi-finished product after the surface drying is placed in a muffle furnace for sintering. The sintering temperature is 835°C and the time is 5 minutes. After the sintering is completed (the coating thickness is 150μM), it is allowed to cool and a common enamel glaze pot is obtained.

[0024] Product Characterization

[0025] Figure 1 This is the SEM image of the nano silver enamel antibacterial pot obtained in Example 1. Figure 1 It can be clearly seen that the silver element is evenly distributed on the surface of the pot.

[0026] Antibacterial performance test

[0027] Test standard: JC / T897-2014.

[0028] Tables 1 and 2 are the test results of antibacterial performance against Staphylococcus aureus and Escherichia coli, respectively, wherein the blank control sample corresponds to the product obtained in Control Example 1, and the antibacterial ceramic sample corresponds to the product obtained in Example 1. It can be seen from Tables 1-2 that the antibacterial rate of the nano-silver enamel glaze antibacterial pot obtained by the present invention against Staphylococcus aureus and Escherichia coli reaches 99.99%, indicating that the present invention has excellent antibacterial performance.

[0029]

[0030]

Claims

1. A method for preparing a nano silver enamel antibacterial device, characterized in that: Here are the steps: (1) Pretreatment: Degreasing the base material of the equipment, after which the surface should be free of wet oil stains and oily dirt; sandblasting after degreasing, after which the roughness should be between 2 and 3 and the surface should be free of obvious brightness and stains; (2) Preparation of antibacterial glaze: (2.1) Prepare enamel slurry according to the conventional formula of enamel glaze; (2.2) The mass parts are measured in g and the volume parts are measured in mL. The nanosilver antibacterial slurry is prepared according to the following steps: (2.2.1) Dissolve 4.6-5 parts by mass of alkyl imidazole in 45-55 parts by volume of water to obtain solution A; (2.2.2), take 60-80 parts by volume of water, add 1.5-2 parts by mass of CTAB, stir at 35-45°C for 30-40 minutes, then add 4.5-5 parts by mass of silver nitrate, then add solution A, then add 10-15 parts by mass of ammonia water, continue stirring for 1-1.5 hours, then drop 6-7 parts by mass of TEOS, continue stirring for 2-2.5 hours, filter it and wash it with water, send the filter cake to dry, grind it after drying, then add ascorbic acid aqueous solution according to the molar ratio of ascorbic acid: silver nitrate = (1.5-3): 1, stir for 0.4-0.7 hours, filter it, add 25-35 parts by volume of water to the filter cake, stir evenly, and obtain nano silver antibacterial slurry; (2.3), mixing the nano-silver antibacterial slurry and the enamel slurry to obtain an antibacterial glaze, based on the mass percentage of silver in the nano-silver antibacterial slurry to the enamel slurry being 0.8-1.2%; (3) Spraying: (3.1) Stir the antibacterial glaze thoroughly before use and keep stirring during use; (3.2) spraying antibacterial glaze on the surface of the utensil substrate obtained after the pretreatment in step (1); (4) Sintering: After the spraying in step (3) is completed, the surface is dried first, and then the semi-finished product after the surface drying is sent for sintering; after the sintering is completed, it is left to cool and the nano silver enamel glaze antibacterial device is obtained.

2. The method for preparing the nano silver enamel antibacterial device according to claim 1, characterized in that: The antibacterial appliances include but are not limited to antibacterial kitchen appliances.

3. The method for preparing the nano silver enamel antibacterial device according to claim 1, characterized in that: In step (2.2.1), the alkyl imidazole is 2-methyl imidazole, 2-ethyl imidazole or 2-propyl imidazole.

4. The method for preparing the nano silver enamel antibacterial device according to claim 1, characterized in that: In step (1), the tool substrate is degreased by high-temperature degreasing, the degreasing temperature is 440-450° C., and the degreasing time is 9-10 minutes.

5. The method for preparing the nano silver enamel antibacterial device according to claim 1, characterized in that: In step (1), during the sandblasting process, 60-80 mesh brown corundum is used and the air pressure is controlled at 4.3-4.7 Pa.

6. The method for preparing the nano silver enamel antibacterial device according to claim 1, characterized in that: In step (2.1), based on the total weight percentage of 100%, the composition of the enamel glaze is 60-63% enamel powder, 4-5% clay, 2-4% iron black, and 30-32% water.

7. The method for preparing the nano silver enamel antibacterial device according to claim 1, characterized in that: In step (2.2.2), the concentration of the ammonia water is 25-28 wt %.

8. The method for preparing the nano silver enamel antibacterial device according to claim 1, characterized in that: In step (3.2), the antibacterial glaze is sprayed with a spray gun. The nozzle diameter of the spray gun is 1.3~1.5mm and it is thoroughly cleaned with water or isopropyl alcohol before use. During spraying, the air pressure is controlled at 3~4.5Pa.

9. The method for preparing the nano silver enamel antibacterial device according to claim 1, characterized in that: In step (4), the surface drying temperature is 140-150°C and the time is 9-10 minutes.

10. The method for preparing the nano silver enamel antibacterial device according to claim 1, characterized in that: In step (4), the sintering temperature is 830-845°C and the sintering time is 4-5 minutes.

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