CN109942208A - A kind of preparation method of antibiotic glass - Google Patents
A kind of preparation method of antibiotic glass Download PDFInfo
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- CN109942208A CN109942208A CN201910211941.2A CN201910211941A CN109942208A CN 109942208 A CN109942208 A CN 109942208A CN 201910211941 A CN201910211941 A CN 201910211941A CN 109942208 A CN109942208 A CN 109942208A
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Abstract
The invention discloses a kind of preparation methods of antibiotic glass, comprising the following steps: cuts glass former material, then carries out finishing impression processing, the pre-heat treatment obtains pretreated glass after cleaning；Heating fusing obtains antibacterial annealing furnace water after potassium nitrate is mixed with silver nitrate, and progress antibacterial tempering in antibacterial annealing furnace water is added in pretreated glass and handles to obtain the antibiotic glass.The preparation method of antibiotic glass proposed by the present invention, process is simple, and obtained antibiotic glass has the characteristic of glass material itself, while good anti-bacterial effect, widely used.
Description
Technical field
The present invention relates to glass technology field more particularly to a kind of preparation methods of antibiotic glass.
Background technique
As domestic more and more people frequently touch mobile phone daily, mobile phone surface can leave many bacteriums, Zeng You
Mechanism detects 10 times dirtier than courier packages unexpectedly of mobile phone.The bacterium that mobile phone surface is largely bred can bring certain danger to human body
Evil.The antibiotic glass that normal glass is processed into can inhibit the growth of the various harmful bacterias such as algae, germ, mould, fungi,
It has been widely used in the fields such as medical care, automobile touch-control and hand-set lid electronic touch product at present.But it is existing anti-
Bacterium antibacterial glass effect is still less desirable, limits its application.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of preparation method of antibiotic glass, processes
Simply, the antibiotic glass obtained has the characteristic of glass material itself, while good anti-bacterial effect, widely used.
A kind of preparation method of antibiotic glass proposed by the present invention, comprising the following steps:
S1, glass former material is cut, then carries out finishing impression processing, the pre-heat treatment obtains pretreated glass after cleaning；
S2, potassium nitrate is mixed with silver nitrate after heating fusing obtain antibacterial annealing furnace water, pretreated glass is added anti-
Antibacterial tempering is carried out in bacterium annealing furnace water to handle to obtain the antibiotic glass.
Preferably, in S1, the temperature of the pre-heat treatment is 340-380 DEG C, time 1-3h.
Preferably, the temperature of the pre-heat treatment is 360 DEG C, time 2h.
Preferably, in S2, the weight ratio of potassium nitrate and silver nitrate is 70-80:0.35-0.4.
Preferably, the weight ratio of potassium nitrate and silver nitrate is 75:0.375.
Preferably, in S2, purity >=99.8wt% of the potassium nitrate；The silver nitrate is to analyze pure silver nitrate.
Preferably, in S2, the temperature of the antibacterial tempering processing is 370-420 DEG C, time 0.5-2h.
Preferably, the temperature of the antibacterial tempering processing is 390 DEG C, time 1h.
It preferably, further include being obtained through antibacterial tempering treated pretreated glass surfaces coating antimicrobial coating in S2
To the antibiotic glass.
Preferably, the raw material of the antimicrobial coating includes: 55-68 parts of polyurethane acrylic resin, 3 the third two by weight
10-21 parts of alcohol diacrylate, 5-12 parts of perluorooctyl acrylate, 2-4 parts of photoinitiator, 3-8 parts of silica solution, polyphenylene sulfide
0.6-2.5 parts, modified Ag-carried nanometer titanium dioxide 5-7 parts, 0.8-3.7 parts of dysprosia, 2-4.6 parts of montmorillonite, γ-mercapto propyl three
0.1-1.3 parts of methoxy silane.
Preferably, the modified Ag-carried nanometer titanium dioxide is prepared according to following technique: by N- carboxymethyl chitosan,
1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride, Quercetin are uniformly mixed with DMSO aqueous solution, and 4- diformazan is added
The pH value of aminopyridine, regulation system is 6-7, and 10-15h is protected from light at 40-45 DEG C, and dehydrated alcohol is then added and stands,
Filtering, is dried to obtain material A at methanol washing；Material A is mixed with acetic acid aqueous solution, 100-250min is stirred at room temperature, is adjusted
Section pH value is 3-4, and allyl glycidyl ether is added, 12-19h is stirred to react at 40-55 DEG C, then heavy with dehydrated alcohol
It forms sediment, is filtered, washed, is dried to obtain material B；Ag-carried nanometer titanium dioxide is added in ethyl alcohol, material B is then added, stirs 30-
It is stood after 50min, is filtered, washed, is dried to obtain the modified Ag-carried nanometer titanium dioxide.
Preferably, in the preparation process of modified Ag-carried nanometer titanium dioxide, mole of N- carboxymethyl chitosan, Quercetin
Than for 1:0.3-0.8；Material A, the weight ratio of allyl glycidyl ether are 3-5:0.2-1；Ag-carried nanometer titanium dioxide, material
The weight ratio of B is 1:2-4.
It is laggard to be processed into desired shape first by the preparation method of antibiotic glass of the present invention for glass-cutting, finishing impression
It has gone the pre-heat treatment, has carried out antibacterial tempering using the mixture of potassium nitrate and silver nitrate later and handled, made by ion exchange
It has been introduced into inside glass with by silver, has assigned the permanent biocidal property of glass, while controlling the weight ratio of potassium nitrate and silver nitrate,
Keep the coloring of gained glass few；Antimicrobial coating is coated on its surface later, wherein the raw material of antimicrobial coating has been specifically chosen poly-
Urethane acrylate resin is performed polymer, while joined perluorooctyl acrylate and tripropylene glycol diacrylate cooperation, is assigned
The excellent water resistance of precoat；In silica solution, polyphenylene sulfide addition system, there is coordinated effect, improve the anti-of coating
Curved intensity and wearability；In the preparation process of modified Ag-carried nanometer titanium dioxide, first using N- carboxymethyl chitosan as raw material,
Under the action of activating reagent 1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine with Mongolian oak
Pi Su is reacted, and is made the hydroxyl in carboxyl and Quercetin in N- carboxymethyl chitosan that esterification have occurred, is obtained
Material A controls the condition of reaction later using material A and allyl glycidyl ether as raw material, makes chitosan molecule in material A
In hydroxyl reacted with allyl glycidyl ether, so that double bond has been introduced into molecule, obtained material B, with
Material B is that modifying agent is modified Ag-carried nanometer titanium dioxide, and material B passes through hydroxyl therein and silver-carrying nano titanium dioxide
Material B has been introduced into the surface of Ag-carried nanometer titanium dioxide by the hydrogen bond action of titanium surface hydroxyl, has obtained modified silver-carrying nano
Titanium dioxide is added into coating, is uniformly dispersed, and avoids its reunion in system, while can participate in the solidification of system,
Its binding force with system is improved, the synergetic antibacterial effect of silver, titanium dioxide, chitosan and Quercetin is played, with glass
In silver ion collaboration, play dual antibacterial action, make gained antibiotic glass antibiotic property it is good, antibacterial timeliness is long；Specific choice
In rare earth oxide dysprosia addition system, unoccupied orbital can form coordinate bond with hydroxyl isopolarity group in system, have
Conducive to the transmitting of energy before group, cooperates with γ-mercaptopropyl trimethoxysilane, accelerate the photo-curing rate of coating, it is double
The mechanical performance of key high conversion rate, coating is excellent, while controlling its content in system, its content is controlled in 0.8-
3.7 parts, it is therefore prevented that its influence that luminous energy is absorbed to photoinitiator ensure that the concentration of living radical in system, while can mention
Rise the anti-microbial property of Ag-carried nanometer titanium dioxide.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of antibiotic glass proposed by the present invention, comprising the following steps:
S1, glass former material is cut, then carries out finishing impression processing, the pre-heat treatment obtains pretreated glass after cleaning；
S2, potassium nitrate is mixed with silver nitrate after heating fusing obtain antibacterial annealing furnace water, pretreated glass is added anti-
Antibacterial tempering is carried out in bacterium annealing furnace water to handle to obtain the antibiotic glass.
Embodiment 2
A kind of preparation method of antibiotic glass proposed by the present invention, comprising the following steps:
S1, glass former material is cut, then carries out finishing impression processing, the pre-heat treatment obtains pretreated glass after cleaning；
S2, potassium nitrate is mixed with silver nitrate after heating fusing obtain antibacterial annealing furnace water, pretreated glass is added anti-
Antibacterial tempering is carried out in bacterium annealing furnace water to handle to obtain the antibiotic glass；
Wherein, in S1, the temperature of the pre-heat treatment is 340 DEG C, time 3h；
In S2, the weight ratio of potassium nitrate and silver nitrate is 80:0.35；
In S2, the purity of the potassium nitrate is 99.8wt%；The silver nitrate is to analyze pure silver nitrate；
In S2, the temperature of the antibacterial tempering processing is 370 DEG C, time 2h.
Embodiment 3
A kind of preparation method of antibiotic glass proposed by the present invention, comprising the following steps:
S1, glass former material is cut, then carries out finishing impression processing, the pre-heat treatment obtains pretreated glass after cleaning；
S2, potassium nitrate is mixed with silver nitrate after heating fusing obtain antibacterial annealing furnace water, pretreated glass is added anti-
Antibacterial tempering is carried out in bacterium annealing furnace water to handle to obtain the antibiotic glass；
Wherein, in S1, the temperature of the pre-heat treatment is 380 DEG C, time 1h；
In S2, the weight ratio of potassium nitrate and silver nitrate is 70:0.4；
In S2, the purity of the potassium nitrate is 99.8wt%；The silver nitrate is to analyze pure silver nitrate；
In S2, the temperature of the antibacterial tempering processing is 420 DEG C, time 0.5h.
Embodiment 4
A kind of preparation method of antibiotic glass proposed by the present invention, comprising the following steps:
S1, glass former material is cut, then carries out finishing impression processing, the pre-heat treatment obtains pretreated glass after cleaning；
S2, potassium nitrate is mixed with silver nitrate after heating fusing obtain antibacterial annealing furnace water, pretreated glass is added anti-
Antibacterial tempering is carried out in bacterium annealing furnace water to handle to obtain the antibiotic glass；
Wherein, in S1, the temperature of the pre-heat treatment is 375 DEG C, time 1.6h；
In S2, the weight ratio of potassium nitrate and silver nitrate is 78:0.36；
In S2, the purity of the potassium nitrate is 99.9wt%；The silver nitrate is to analyze pure silver nitrate；
In S2, the temperature of the antibacterial tempering processing is 378 DEG C, time 1.7h；
In S2, further include obtained through antibacterial tempering treated pretreated glass surfaces coating antimicrobial coating it is described anti-
Bacterium glass；
The raw material of the antimicrobial coating includes: 55 parts of polyurethane acrylic resin, tripropylene glycol diacrylate by weight
21 parts of ester, 5 parts of perluorooctyl acrylate, 4 parts of photoinitiator, 3 parts of silica solution, 2.5 parts of polyphenylene sulfide, modified silver-carrying nano two
5 parts of titanium oxide, 3.7 parts of dysprosia, 2 parts of montmorillonite, 1.3 parts of γ-mercaptopropyl trimethoxysilane；
The modified Ag-carried nanometer titanium dioxide is prepared according to following technique: by N- carboxymethyl chitosan, 1- ethyl-
(3- dimethylaminopropyl) carbodiimide hydrochloride, Quercetin are uniformly mixed with DMSO aqueous solution, and 4- dimethylamino pyrrole is added
Pyridine, the pH value of regulation system are 6, and 10h is protected from light at 45 DEG C, and dehydrated alcohol is then added and stands, filtering, methanol washing,
It is dried to obtain material A；Material A is mixed with acetic acid aqueous solution, 250min is stirred at room temperature, adjusting pH value is 3, and allyl is added
Base glycidol ether is stirred to react 12h at 55 DEG C, is then precipitated with dehydrated alcohol, is filtered, washed, is dried to obtain material B；
Ag-carried nanometer titanium dioxide is added in ethyl alcohol, material B is then added, is stood after stirring 50min, is filtered, washed, is dried to obtain
The modified Ag-carried nanometer titanium dioxide；
In the preparation process of modified Ag-carried nanometer titanium dioxide, N- carboxymethyl chitosan, Quercetin molar ratio be 1:
0.3；Material A, the weight ratio of allyl glycidyl ether are 5:0.2；Ag-carried nanometer titanium dioxide, material B weight ratio be 1:
4。
Embodiment 5
A kind of preparation method of antibiotic glass proposed by the present invention, comprising the following steps:
S1, glass former material is cut, then carries out finishing impression processing, the pre-heat treatment obtains pretreated glass after cleaning；
S2, potassium nitrate is mixed with silver nitrate after heating fusing obtain antibacterial annealing furnace water, pretreated glass is added anti-
Antibacterial tempering is carried out in bacterium annealing furnace water to handle to obtain the antibiotic glass；
Wherein, in S1, the temperature of the pre-heat treatment is 346 DEG C, time 2.7h；
In S2, the weight ratio of potassium nitrate and silver nitrate is 72:0.39；
In S2, the purity of the potassium nitrate is 99.8wt%；The silver nitrate is to analyze pure silver nitrate；
In S2, the temperature of the antibacterial tempering processing is 410 DEG C, time 0.9h；
In S2, further include obtained through antibacterial tempering treated pretreated glass surfaces coating antimicrobial coating it is described anti-
Bacterium glass；
The raw material of the antimicrobial coating includes: 68 parts of polyurethane acrylic resin, tripropylene glycol diacrylate by weight
10 parts of ester, 12 parts of perluorooctyl acrylate, 2 parts of photoinitiator, 8 parts of silica solution, 0.6 part of polyphenylene sulfide, modified silver-carrying nano
7 parts of titanium dioxide, 0.8 part of dysprosia, 4.6 parts of montmorillonite, 0.1 part of γ-mercaptopropyl trimethoxysilane；
The modified Ag-carried nanometer titanium dioxide is prepared according to following technique: by N- carboxymethyl chitosan, 1- ethyl-
(3- dimethylaminopropyl) carbodiimide hydrochloride, Quercetin are uniformly mixed with DMSO aqueous solution, and 4- dimethylamino pyrrole is added
Pyridine, the pH value of regulation system are 7, and 15h is protected from light at 40 DEG C, and dehydrated alcohol is then added and stands, filtering, methanol washing,
It is dried to obtain material A；Material A is mixed with acetic acid aqueous solution, 100min is stirred at room temperature, adjusting pH value is 4, and allyl is added
Base glycidol ether is stirred to react 19h at 40 DEG C, is then precipitated with dehydrated alcohol, is filtered, washed, is dried to obtain material B；
Ag-carried nanometer titanium dioxide is added in ethyl alcohol, material B is then added, is stood after stirring 30min, is filtered, washed, is dried to obtain
The modified Ag-carried nanometer titanium dioxide；
In the preparation process of modified Ag-carried nanometer titanium dioxide, N- carboxymethyl chitosan, Quercetin molar ratio be 1:
0.8；Material A, the weight ratio of allyl glycidyl ether are 3:1；Ag-carried nanometer titanium dioxide, material B weight ratio be 1:2.
Embodiment 6
A kind of preparation method of antibiotic glass proposed by the present invention, comprising the following steps:
S1, glass former material is cut, then carries out finishing impression processing, the pre-heat treatment obtains pretreated glass after cleaning；
S2, potassium nitrate is mixed with silver nitrate after heating fusing obtain antibacterial annealing furnace water, pretreated glass is added anti-
Antibacterial tempering is carried out in bacterium annealing furnace water to handle to obtain the antibiotic glass；
Wherein, in S1, the temperature of the pre-heat treatment is 360 DEG C, time 2h；
In S2, the weight ratio of potassium nitrate and silver nitrate is 75:0.375；
In S2, the purity of the potassium nitrate is 99.8wt%；The silver nitrate is to analyze pure silver nitrate；
In S2, the temperature of the antibacterial tempering processing is 390 DEG C, time 1h；
In S2, further include obtained through antibacterial tempering treated pretreated glass surfaces coating antimicrobial coating it is described anti-
Bacterium glass；
The raw material of the antimicrobial coating includes: 65 parts of polyurethane acrylic resin, tripropylene glycol diacrylate by weight
16 parts of ester, 7 parts of perluorooctyl acrylate, 3 parts of photoinitiator, 6 parts of silica solution, 2 parts of polyphenylene sulfide, modified silver-carrying nano dioxy
Change 5.8 parts of titanium, 3 parts of dysprosia, 2.9 parts of montmorillonite, 0.7 part of γ-mercaptopropyl trimethoxysilane；
The modified Ag-carried nanometer titanium dioxide is prepared according to following technique: by N- carboxymethyl chitosan, 1- ethyl-
(3- dimethylaminopropyl) carbodiimide hydrochloride, Quercetin are uniformly mixed with DMSO aqueous solution, and 4- dimethylamino pyrrole is added
Pyridine, the pH value of regulation system are 6, and 12h is protected from light at 43 DEG C, and dehydrated alcohol is then added and stands, filtering, methanol washing,
It is dried to obtain material A；Material A is mixed with acetic acid aqueous solution, 200min is stirred at room temperature, adjusting pH value is 3.5, and alkene is added
Propyl glycidyl ether is stirred to react 15h at 50 DEG C, is then precipitated with dehydrated alcohol, is filtered, washed, is dried to obtain material
B；Ag-carried nanometer titanium dioxide is added in ethyl alcohol, material B is then added, is stood after stirring 40min, is filtered, washed, dries
To the modified Ag-carried nanometer titanium dioxide；
In the preparation process of modified Ag-carried nanometer titanium dioxide, N- carboxymethyl chitosan, Quercetin molar ratio be 1:
0.6；Material A, the weight ratio of allyl glycidyl ether are 4:0.7；Ag-carried nanometer titanium dioxide, material B weight ratio be 1:
3。
The antibiotic glass prepared to embodiment 2 detects, and wherein the content of Ag is that (limit standard is 644.40ppm
1000.00ppm), content silver-colored in simple glass is 0.
Performance detection carried out to the antibiotic glass for preparing in embodiment 1-3, CS value 804.357-814.086MPa it
Between, DOL value is between 46.092-48.736 μm, and CT value is between 61.514-65.481MPa.
To the antibiotic glass and existing simple glass progress performance detection in embodiment 1-3, testing result such as following table
It is shown:
As seen from the above table, the bending resistance of antibiotic glass is excellent.
Performance detection is carried out to embodiment 1-3 and simple glass, as a result as shown in the table:
As seen from the above table, the impact resistance of antibiotic glass is good.
According to the standard of JC/T 1054-2007 plated film antibiotic glass to the embodiment 3-6 antibiotic glass prepared and existing
The antibiotic property of glass detected, wherein test strain is Escherichia coli and staphylococcus aureus；After tested it is found that implementing
Antibiotic glass obtained by example 4-6 reaches 99.999% or more to the antibiotic rate of Escherichia coli and staphylococcus aureus, embodiment 3
The antibiotic glass of preparation is 98.68% to the antibiotic rate of Escherichia coli, and the antibiotic rate to staphylococcus aureus is 99.27%,
And existing glass is 89.38% to the antibiotic rate of Escherichia coli, the antibiotic rate to staphylococcus aureus is 90.12%.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of antibiotic glass, which comprises the following steps:
S1, glass former material is cut, then carries out finishing impression processing, the pre-heat treatment obtains pretreated glass after cleaning；
S2, potassium nitrate is mixed with silver nitrate after heating fusing obtain antibacterial annealing furnace water, by pretreated glass be added antibacterial steel
Change progress antibacterial tempering in furnace water to handle to obtain the antibiotic glass.
2. the preparation method of antibiotic glass according to claim 1, which is characterized in that in S1, the temperature of the pre-heat treatment
Degree is 340-380 DEG C, time 1-3h；Preferably, the temperature of the pre-heat treatment is 360 DEG C, time 2h.
3. the preparation method of antibiotic glass according to claim 1 or claim 2, which is characterized in that in S2, potassium nitrate and silver nitrate
Weight ratio be 70-80:0.35-0.4；Preferably, the weight ratio of potassium nitrate and silver nitrate is 75:0.375.
4. the preparation method of antibiotic glass described in any one of -3 according to claim 1, which is characterized in that in S2, the nitre
Purity >=99.8wt% of sour potassium；The silver nitrate is to analyze pure silver nitrate.
5. the preparation method of antibiotic glass described in any one of -4 according to claim 1, which is characterized in that described anti-in S2
The temperature of bacterium tempering processing is 370-420 DEG C, time 0.5-2h；Preferably, the temperature of the antibacterial tempering processing is 390
DEG C, time 1h.
6. the preparation method of antibiotic glass described in any one of -5 according to claim 1, which is characterized in that in S2, further include
The antibiotic glass is being obtained through antibacterial tempering treated pretreated glass surfaces coating antimicrobial coating.
7. the preparation method of antibiotic glass according to claim 6, which is characterized in that the raw material of the antimicrobial coating is by weight
Part includes: 55-68 parts of polyurethane acrylic resin, 10-21 parts of tripropylene glycol diacrylate, perluorooctyl acrylate 5-12
Part, 2-4 parts of photoinitiator, 3-8 parts of silica solution, 0.6-2.5 parts of polyphenylene sulfide, Ag-carried nanometer titanium dioxide 5-7 parts modified, oxidation
0.8-3.7 parts of dysprosium, 2-4.6 parts of montmorillonite, 0.1-1.3 parts of γ-mercaptopropyl trimethoxysilane.
8. the preparation method of antibiotic glass according to claim 7, which is characterized in that the modified Ag-carried nanometer titanium dioxide
It is prepared according to following technique: by N- carboxymethyl chitosan, 1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride
Salt, Quercetin are uniformly mixed with DMSO aqueous solution, 4-dimethylaminopyridine are added, the pH value of regulation system is 6-7, in 40-45
It is protected from light 10-15h at DEG C, dehydrated alcohol is then added and stands, filtering, is dried to obtain material A at methanol washing；By material A with
100-250min is stirred at room temperature in acetic acid aqueous solution mixing, and adjusting pH value is 3-4, and allyl glycidyl ether is added,
It is stirred to react 12-19h at 40-55 DEG C, is then precipitated with dehydrated alcohol, is filtered, washed, is dried to obtain material B；By silver-carrying nano
Titanium dioxide is added in ethyl alcohol, and material B is then added, and stands after stirring 30-50min, is filtered, washed, is dried to obtain described change
Property Ag-carried nanometer titanium dioxide.
9. the preparation method of antibiotic glass according to claim 8, which is characterized in that in modified Ag-carried nanometer titanium dioxide
In preparation process, N- carboxymethyl chitosan, Quercetin molar ratio be 1:0.3-0.8；Material A, allyl glycidyl ether
Weight ratio is 3-5:0.2-1；Ag-carried nanometer titanium dioxide, material B weight ratio be 1:2-4.
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| US11560487B2 (en) | 2020-09-22 | 2023-01-24 | Swimc Llc | Coating compositions containing low molecular weight chitosan composition |
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| CN109942208B (en) | 2022-03-18 |
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