CN109942208B - Preparation method of antibacterial glass - Google Patents
Preparation method of antibacterial glass Download PDFInfo
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- CN109942208B CN109942208B CN201910211941.2A CN201910211941A CN109942208B CN 109942208 B CN109942208 B CN 109942208B CN 201910211941 A CN201910211941 A CN 201910211941A CN 109942208 B CN109942208 B CN 109942208B
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Abstract
The invention discloses a preparation method of antibacterial glass, which comprises the following steps: cutting a glass raw material, then carrying out fine carving processing, cleaning, and carrying out preheating treatment to obtain pretreated glass; mixing potassium nitrate and silver nitrate, heating and melting to obtain antibacterial tempering furnace water, and adding the pretreated glass into the antibacterial tempering furnace water for antibacterial tempering treatment to obtain the antibacterial glass. The preparation method of the antibacterial glass provided by the invention has the advantages that the process is simple, the obtained antibacterial glass has the characteristics of glass materials, and meanwhile, the antibacterial effect is good, and the application is wide.
Description
Technical Field
The invention relates to the technical field of glass, in particular to a preparation method of antibacterial glass.
Background
With more and more people in development China frequently touch the mobile phone every day, a lot of bacteria are left on the surface of the mobile phone, and the organization has ever detected that the mobile phone is 10 times dirtier than an express package. The large amount of bacteria on the surface of the mobile phone can bring certain harm to the human body. The antibacterial glass processed from the normal glass can inhibit the breeding of various harmful bacteria such as algae, microbe, mildew, fungi and the like, and is widely applied to the fields of medical care, automobile touch, mobile phone cover plate electronic touch products and the like at present. However, the antibacterial effect of the existing antibacterial glass is still not ideal, and the application of the existing antibacterial glass is limited.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the preparation method of the antibacterial glass, the process is simple, the obtained antibacterial glass has the characteristics of glass materials, and meanwhile, the antibacterial glass has a good antibacterial effect and wide application.
The invention provides a preparation method of antibacterial glass, which comprises the following steps:
s1, cutting the glass raw material, then carrying out fine carving processing, cleaning and preheating to obtain pretreated glass;
and S2, mixing potassium nitrate and silver nitrate, heating and melting to obtain antibacterial tempering furnace water, and adding the pretreated glass into the antibacterial tempering furnace water for antibacterial tempering treatment to obtain the antibacterial glass.
Preferably, in S1, the temperature of the preheating treatment is 340-380 ℃ and the time is 1-3 h.
Preferably, the temperature of the preheating treatment is 360 ℃ and the time is 2 h.
Preferably, in S2, the weight ratio of potassium nitrate to silver nitrate is 70-80: 0.35-0.4.
Preferably, the weight ratio of potassium nitrate to silver nitrate is 75: 0.375.
preferably, in S2, the purity of the potassium nitrate is more than or equal to 99.8 wt%; the silver nitrate is analytically pure silver nitrate.
Preferably, in S2, the temperature of the antibacterial tempering treatment is 370-420 ℃, and the time is 0.5-2 h.
Preferably, the temperature of the antibacterial tempering treatment is 390 ℃, and the time is 1 h.
Preferably, in S2, the method further includes applying an antibacterial coating on the surface of the pretreated glass after the antibacterial tempering treatment to obtain the antibacterial glass.
Preferably, the raw materials of the antibacterial coating comprise, by weight: 55-68 parts of polyurethane acrylic resin, 10-21 parts of tripropylene glycol diacrylate, 5-12 parts of tridecafluorooctyl acrylate, 2-4 parts of photoinitiator, 3-8 parts of silica sol, 0.6-2.5 parts of polyphenylene sulfide, 5-7 parts of modified silver-loaded nano titanium dioxide, 0.8-3.7 parts of dysprosium oxide, 2-4.6 parts of montmorillonite and 0.1-1.3 parts of gamma-mercaptopropyl trimethoxy silane.
Preferably, the modified silver-loaded nano titanium dioxide is prepared according to the following process: uniformly mixing N-carboxymethyl chitosan, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, quercetin and a DMSO (dimethyl sulfoxide) aqueous solution, adding 4-dimethylaminopyridine, adjusting the pH value of a system to be 6-7, reacting for 10-15h at 40-45 ℃ in a dark place, then adding absolute ethyl alcohol, standing, filtering, washing with methanol, and drying to obtain a material A; mixing the material A with an acetic acid aqueous solution, stirring at room temperature for 100-250min, adjusting the pH value to 3-4, adding allyl glycidyl ether, stirring and reacting at 40-55 ℃ for 12-19h, then precipitating with absolute ethyl alcohol, filtering, washing and drying to obtain a material B; adding the silver-loaded nano titanium dioxide into ethanol, then adding the material B, stirring for 30-50min, standing, filtering, washing and drying to obtain the modified silver-loaded nano titanium dioxide.
Preferably, in the preparation process of the modified silver-loaded nano titanium dioxide, the molar ratio of the N-carboxymethyl chitosan to the quercetin is 1: 0.3-0.8; the weight ratio of the material A to the allyl glycidyl ether is 3-5: 0.2 to 1; the weight ratio of the silver-loaded nano titanium dioxide to the material B is 1: 2-4.
According to the preparation method of the antibacterial glass, firstly, the glass is cut and carved into a desired shape, then preheating treatment is carried out, then antibacterial tempering treatment is carried out by utilizing a mixture of potassium nitrate and silver nitrate, silver is introduced into the glass through ion exchange, the glass is endowed with permanent antibacterial activity, and meanwhile, the weight ratio of the potassium nitrate to the silver nitrate is controlled, so that the obtained glass is less colored; then an antibacterial coating is coated on the surface of the antibacterial coating, wherein polyurethane acrylic resin is specifically selected as a prepolymer as a raw material of the antibacterial coating, and tridecyl octyl acrylate and tripropylene glycol diacrylate are added for matching, so that the coating is endowed with excellent water resistance; the silica sol and the polyphenylene sulfide are added into the system, so that the synergistic effect is achieved, and the bending strength and the wear resistance of the coating are improved; in the preparation process of the modified silver-carrying nano titanium dioxide, N-carboxymethyl chitosan is firstly used as a raw material and reacts with quercetin under the action of an activating reagent 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine to enable carboxyl in the N-carboxymethyl chitosan and hydroxyl in the quercetin to generate esterification reaction to obtain a material A, then the material A and allyl glycidyl ether are used as raw materials, the reaction conditions are controlled to enable the hydroxyl in chitosan molecules in the material A and the allyl glycidyl ether to generate reaction, so that double bonds are introduced into the molecules to obtain a material B, the material B is used as a modifying agent to modify the silver-carrying nano titanium dioxide, and the material B is subjected to hydrogen bond interaction between the hydroxyl in the material and the hydroxyl on the surface of the silver-carrying nano titanium dioxide, introducing the material B onto the surface of the silver-loaded nano titanium dioxide to obtain modified silver-loaded nano titanium dioxide, adding the modified silver-loaded nano titanium dioxide into the coating, dispersing uniformly, avoiding agglomeration of the modified silver-loaded nano titanium dioxide in a system, simultaneously participating in curing of the system, improving the binding force of the modified silver-loaded nano titanium dioxide and the system, exerting the synergistic antibacterial action of silver, titanium dioxide, chitosan and quercetin, and exerting dual antibacterial action by cooperating with silver ions in glass, so that the obtained antibacterial glass has good antibacterial property and long antibacterial aging; the rare earth oxide dysprosium oxide is added into the system, the vacant orbit of the dysprosium oxide can form a coordination bond with polar groups such as hydroxyl groups in the system, energy transfer before the groups is facilitated, the dysprosium oxide is matched with gamma-mercaptopropyl trimethoxysilane, so that the photocuring rate of the coating is accelerated, the conversion rate of double bonds is high, the mechanical property of the coating is excellent, the content of the dysprosium oxide in the system is controlled to be 0.8-3.7 parts, the influence of the dysprosium oxide on the light absorption energy of a photoinitiator is prevented, the concentration of active free radicals in the system is ensured, and the antibacterial property of the silver-loaded nano titanium dioxide can be improved.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
The invention provides a preparation method of antibacterial glass, which comprises the following steps:
s1, cutting the glass raw material, then carrying out fine carving processing, cleaning and preheating to obtain pretreated glass;
and S2, mixing potassium nitrate and silver nitrate, heating and melting to obtain antibacterial tempering furnace water, and adding the pretreated glass into the antibacterial tempering furnace water for antibacterial tempering treatment to obtain the antibacterial glass.
Example 2
The invention provides a preparation method of antibacterial glass, which comprises the following steps:
s1, cutting the glass raw material, then carrying out fine carving processing, cleaning and preheating to obtain pretreated glass;
s2, mixing potassium nitrate and silver nitrate, heating and melting to obtain antibacterial tempering furnace water, and adding the pretreated glass into the antibacterial tempering furnace water for antibacterial tempering treatment to obtain the antibacterial glass;
wherein in S1, the temperature of the preheating treatment is 340 ℃, and the time is 3 h;
in S2, the weight ratio of potassium nitrate to silver nitrate is 80: 0.35;
in S2, the potassium nitrate has a purity of 99.8 wt%; the silver nitrate is analytically pure silver nitrate;
in S2, the temperature of the antibacterial tempering treatment is 370 ℃, and the time is 2 h.
Example 3
The invention provides a preparation method of antibacterial glass, which comprises the following steps:
s1, cutting the glass raw material, then carrying out fine carving processing, cleaning and preheating to obtain pretreated glass;
s2, mixing potassium nitrate and silver nitrate, heating and melting to obtain antibacterial tempering furnace water, and adding the pretreated glass into the antibacterial tempering furnace water for antibacterial tempering treatment to obtain the antibacterial glass;
wherein in S1, the temperature of the preheating treatment is 380 ℃ and the time is 1 h;
in S2, the weight ratio of potassium nitrate to silver nitrate is 70: 0.4;
in S2, the potassium nitrate has a purity of 99.8 wt%; the silver nitrate is analytically pure silver nitrate;
in S2, the temperature of the antibacterial tempering treatment is 420 ℃, and the time is 0.5 h.
Example 4
The invention provides a preparation method of antibacterial glass, which comprises the following steps:
s1, cutting the glass raw material, then carrying out fine carving processing, cleaning and preheating to obtain pretreated glass;
s2, mixing potassium nitrate and silver nitrate, heating and melting to obtain antibacterial tempering furnace water, and adding the pretreated glass into the antibacterial tempering furnace water for antibacterial tempering treatment to obtain the antibacterial glass;
wherein in S1, the temperature of the preheating treatment is 375 ℃, and the time is 1.6 h;
in S2, the weight ratio of potassium nitrate to silver nitrate is 78: 0.36;
in S2, the potassium nitrate has a purity of 99.9 wt%; the silver nitrate is analytically pure silver nitrate;
in S2, the temperature of the antibacterial tempering treatment is 378 ℃ and the time is 1.7 h;
in S2, coating an antibacterial coating on the surface of the pretreated glass subjected to the antibacterial tempering treatment to obtain the antibacterial glass;
the antibacterial coating comprises the following raw materials in parts by weight: 55 parts of polyurethane acrylic resin, 21 parts of tripropylene glycol diacrylate, 5 parts of tridecyl acrylate, 4 parts of photoinitiator, 3 parts of silica sol, 2.5 parts of polyphenylene sulfide, 5 parts of modified silver-loaded nano titanium dioxide, 3.7 parts of dysprosium oxide, 2 parts of montmorillonite and 1.3 parts of gamma-mercaptopropyl trimethoxy silane;
the modified silver-loaded nano titanium dioxide is prepared according to the following process: uniformly mixing N-carboxymethyl chitosan, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, quercetin and a DMSO (dimethyl sulfoxide) aqueous solution, adding 4-dimethylaminopyridine, adjusting the pH value of a system to be 6, reacting for 10 hours at 45 ℃ in a dark place, adding absolute ethyl alcohol, standing, filtering, washing with methanol, and drying to obtain a material A; mixing the material A with an acetic acid aqueous solution, stirring at room temperature for 250min, adjusting the pH value to 3, adding allyl glycidyl ether, stirring at 55 ℃ for reaction for 12h, then precipitating with absolute ethanol, filtering, washing and drying to obtain a material B; adding silver-loaded nano titanium dioxide into ethanol, then adding the material B, stirring for 50min, standing, filtering, washing and drying to obtain the modified silver-loaded nano titanium dioxide;
in the preparation process of the modified silver-loaded nano titanium dioxide, the molar ratio of the N-carboxymethyl chitosan to the quercetin is 1: 0.3; the weight ratio of the material A to the allyl glycidyl ether is 5: 0.2; the weight ratio of the silver-loaded nano titanium dioxide to the material B is 1: 4.
example 5
The invention provides a preparation method of antibacterial glass, which comprises the following steps:
s1, cutting the glass raw material, then carrying out fine carving processing, cleaning and preheating to obtain pretreated glass;
s2, mixing potassium nitrate and silver nitrate, heating and melting to obtain antibacterial tempering furnace water, and adding the pretreated glass into the antibacterial tempering furnace water for antibacterial tempering treatment to obtain the antibacterial glass;
wherein in S1, the temperature of the preheating treatment is 346 ℃, and the time is 2.7 h;
in S2, the weight ratio of potassium nitrate to silver nitrate is 72: 0.39;
in S2, the potassium nitrate has a purity of 99.8 wt%; the silver nitrate is analytically pure silver nitrate;
in S2, the temperature of the antibacterial tempering treatment is 410 ℃, and the time is 0.9 h;
in S2, coating an antibacterial coating on the surface of the pretreated glass subjected to the antibacterial tempering treatment to obtain the antibacterial glass;
the antibacterial coating comprises the following raw materials in parts by weight: 68 parts of polyurethane acrylic resin, 10 parts of tripropylene glycol diacrylate, 12 parts of tridecyl octyl acrylate, 2 parts of photoinitiator, 8 parts of silica sol, 0.6 part of polyphenylene sulfide, 7 parts of modified silver-loaded nano titanium dioxide, 0.8 part of dysprosium oxide, 4.6 parts of montmorillonite and 0.1 part of gamma-mercaptopropyl trimethoxy silane;
the modified silver-loaded nano titanium dioxide is prepared according to the following process: uniformly mixing N-carboxymethyl chitosan, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, quercetin and a DMSO (dimethyl sulfoxide) aqueous solution, adding 4-dimethylaminopyridine, adjusting the pH value of a system to be 7, reacting for 15 hours at 40 ℃ in a dark place, adding absolute ethyl alcohol, standing, filtering, washing with methanol, and drying to obtain a material A; mixing the material A with an acetic acid aqueous solution, stirring at room temperature for 100min, adjusting the pH value to 4, adding allyl glycidyl ether, stirring at 40 ℃ for reacting for 19h, then precipitating with absolute ethanol, filtering, washing and drying to obtain a material B; adding silver-loaded nano titanium dioxide into ethanol, then adding the material B, stirring for 30min, standing, filtering, washing and drying to obtain the modified silver-loaded nano titanium dioxide;
in the preparation process of the modified silver-loaded nano titanium dioxide, the molar ratio of the N-carboxymethyl chitosan to the quercetin is 1: 0.8; the weight ratio of the material A to the allyl glycidyl ether is 3: 1; the weight ratio of the silver-loaded nano titanium dioxide to the material B is 1: 2.
example 6
The invention provides a preparation method of antibacterial glass, which comprises the following steps:
s1, cutting the glass raw material, then carrying out fine carving processing, cleaning and preheating to obtain pretreated glass;
s2, mixing potassium nitrate and silver nitrate, heating and melting to obtain antibacterial tempering furnace water, and adding the pretreated glass into the antibacterial tempering furnace water for antibacterial tempering treatment to obtain the antibacterial glass;
wherein in S1, the temperature of the preheating treatment is 360 ℃ and the time is 2 h;
in S2, the weight ratio of potassium nitrate to silver nitrate is 75: 0.375;
in S2, the potassium nitrate has a purity of 99.8 wt%; the silver nitrate is analytically pure silver nitrate;
in S2, the temperature of the antibacterial tempering treatment is 390 ℃, and the time is 1 h;
in S2, coating an antibacterial coating on the surface of the pretreated glass subjected to the antibacterial tempering treatment to obtain the antibacterial glass;
the antibacterial coating comprises the following raw materials in parts by weight: 65 parts of polyurethane acrylic resin, 16 parts of tripropylene glycol diacrylate, 7 parts of tridecyl acrylate, 3 parts of photoinitiator, 6 parts of silica sol, 2 parts of polyphenylene sulfide, 5.8 parts of modified silver-loaded nano titanium dioxide, 3 parts of dysprosium oxide, 2.9 parts of montmorillonite and 0.7 part of gamma-mercaptopropyl trimethoxy silane;
the modified silver-loaded nano titanium dioxide is prepared according to the following process: uniformly mixing N-carboxymethyl chitosan, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, quercetin and a DMSO (dimethyl sulfoxide) aqueous solution, adding 4-dimethylaminopyridine, adjusting the pH value of a system to be 6, reacting for 12 hours at 43 ℃ in a dark place, adding absolute ethyl alcohol, standing, filtering, washing with methanol, and drying to obtain a material A; mixing the material A with an acetic acid aqueous solution, stirring at room temperature for 200min, adjusting the pH value to 3.5, adding allyl glycidyl ether, stirring at 50 ℃ for reaction for 15h, then precipitating with absolute ethyl alcohol, filtering, washing and drying to obtain a material B; adding silver-loaded nano titanium dioxide into ethanol, then adding the material B, stirring for 40min, standing, filtering, washing and drying to obtain the modified silver-loaded nano titanium dioxide;
in the preparation process of the modified silver-loaded nano titanium dioxide, the molar ratio of the N-carboxymethyl chitosan to the quercetin is 1: 0.6; the weight ratio of the material A to the allyl glycidyl ether is 4: 0.7; the weight ratio of the silver-loaded nano titanium dioxide to the material B is 1: 3.
the antibacterial glass prepared in example 2 was examined, wherein the content of Ag was 644.40ppm (defined standard was 1000.00ppm), and the content of silver in the general glass was 0.
The antibacterial glass prepared in the examples 1 to 3 is subjected to performance detection, and the CS value is 804.357-814.086MPa, the DOL value is 46.092-48.736 mu m, and the CT value is 61.514-65.481 MPa.
The antibacterial glass in examples 1 to 3 and the conventional ordinary glass were subjected to performance tests, and the test results are shown in the following table:
as can be seen from the above table, the antibacterial glass is excellent in bending resistance.
The results of the performance tests performed on examples 1 to 3 and on the conventional glass are shown in the following table:
as can be seen from the above table, the antibacterial glass has good impact resistance.
The antibacterial properties of the antibacterial glass prepared in the examples 3-6 and the existing glass are detected according to the standard of JC/T1054-2007 coating antibacterial glass, wherein the test strains are escherichia coli and staphylococcus aureus; tests show that the antibacterial rate of the antibacterial glass obtained in the examples 4-6 to escherichia coli and staphylococcus aureus reaches more than 99.999%, the antibacterial rate of the antibacterial glass prepared in the example 3 to escherichia coli is 98.68%, the antibacterial rate to staphylococcus aureus is 99.27%, the antibacterial rate of the existing glass to escherichia coli is 89.38%, and the antibacterial rate to staphylococcus aureus is 90.12%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. The preparation method of the antibacterial glass is characterized by comprising the following steps:
s1, cutting the glass raw material, then carrying out fine carving processing, cleaning and preheating to obtain pretreated glass;
s2, mixing potassium nitrate and silver nitrate, heating and melting to obtain antibacterial tempering furnace water, and adding the pretreated glass into the antibacterial tempering furnace water for antibacterial tempering treatment to obtain the antibacterial glass; coating an antibacterial coating on the surface of the pretreated glass subjected to the antibacterial tempering treatment to obtain the antibacterial glass; the antibacterial coating comprises the following raw materials in parts by weight: 55-68 parts of polyurethane acrylic resin, 10-21 parts of tripropylene glycol diacrylate, 5-12 parts of tridecafluorooctyl acrylate, 2-4 parts of photoinitiator, 3-8 parts of silica sol, 0.6-2.5 parts of polyphenylene sulfide, 5-7 parts of modified silver-loaded nano titanium dioxide, 0.8-3.7 parts of dysprosium oxide, 2-4.6 parts of montmorillonite and 0.1-1.3 parts of gamma-mercaptopropyl trimethoxy silane;
the modified silver-loaded nano titanium dioxide is prepared according to the following process: uniformly mixing N-carboxymethyl chitosan, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, quercetin and a DMSO (dimethyl sulfoxide) aqueous solution, adding 4-dimethylaminopyridine, adjusting the pH value of a system to be 6-7, reacting for 10-15h at 40-45 ℃ in a dark place, then adding absolute ethyl alcohol, standing, filtering, washing with methanol, and drying to obtain a material A; mixing the material A with an acetic acid aqueous solution, stirring at room temperature for 100-250min, adjusting the pH value to 3-4, adding allyl glycidyl ether, stirring and reacting at 40-55 ℃ for 12-19h, then precipitating with absolute ethyl alcohol, filtering, washing and drying to obtain a material B; adding the silver-loaded nano titanium dioxide into ethanol, then adding the material B, stirring for 30-50min, standing, filtering, washing and drying to obtain the modified silver-loaded nano titanium dioxide.
2. The method as claimed in claim 1, wherein the preheating treatment is performed at 380 ℃ for 1-3h in S1.
3. The method for producing an antibacterial glass according to claim 1 or 2, wherein in S2, the weight ratio of potassium nitrate to silver nitrate is 70 to 80: 0.35-0.4.
4. The method for producing antibacterial glass according to claim 1, wherein in S2, the purity of potassium nitrate is not less than 99.8 wt%; the silver nitrate is analytically pure silver nitrate.
5. The method for preparing the antibacterial glass according to claim 1, wherein in S2, the temperature of the antibacterial tempering treatment is 370-420 ℃, and the time is 0.5-2 h.
6. The method for preparing antibacterial glass according to claim 1, wherein in the preparation process of the modified silver-loaded nano titanium dioxide, the molar ratio of the N-carboxymethyl chitosan to the quercetin is 1: 0.3-0.8; the weight ratio of the material A to the allyl glycidyl ether is 3-5: 0.2 to 1; the weight ratio of the silver-loaded nano titanium dioxide to the material B is 1: 2-4.
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| CN111499220B (en) * | 2020-04-24 | 2022-07-08 | 东莞市冠和光学玻璃有限公司 | Preparation method of antibacterial glass applied to handheld electronic equipment and antibacterial glass |
| EP4217432A1 (en) | 2020-09-22 | 2023-08-02 | Swimc Llc | Chitosan-containing coating compositions |
| CN112299731B (en) * | 2020-10-21 | 2022-05-27 | 同曦集团有限公司 | Colorless transparent antibacterial glass and preparation method thereof |
| CN113321428B (en) * | 2021-05-26 | 2023-05-09 | 胡波 | Antibacterial glass product and preparation method thereof |
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