CN111567556A - Modified nano Ag-doped epoxy resin antibacterial material and preparation method thereof - Google Patents
Modified nano Ag-doped epoxy resin antibacterial material and preparation method thereof Download PDFInfo
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- CN111567556A CN111567556A CN202010637345.3A CN202010637345A CN111567556A CN 111567556 A CN111567556 A CN 111567556A CN 202010637345 A CN202010637345 A CN 202010637345A CN 111567556 A CN111567556 A CN 111567556A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
Abstract
The invention relates to the technical field of antibacterial materials and discloses a modified nano Ag-doped epoxy resin antibacterial material, polydopamine nano-particles contain rich phenolic hydroxyl groups, can delay the ultraviolet light degradation of the antibacterial material, the polydopamine nano-particles contain rich phenolic hydroxyl and quinone groups, can chelate silver ions and reduce the silver ions into nano simple substance silver, the nano silver has higher catalytic capability, so that atomic oxygen with strong oxidizing property is generated in the surrounding space, can effectively sterilize, the polymer functionalized nano Ag is doped with polydopamine nano particles, a large amount of amino groups are introduced on the surface, the epoxy resin and the epoxy resin are subjected to cross-linking reaction, so that the epoxy resin has excellent antibacterial property and ageing resistance, meanwhile, a chemical bond is formed, so that the high-molecular functionalized nano Ag doped polydopamine nano particles limit the chain segment movement of the epoxy resin, and the thermal stability of the composite material is improved.
Description
Technical Field
The invention relates to the technical field of antibacterial materials, in particular to a modified nano Ag-doped epoxy resin antibacterial material and a preparation method thereof.
Background
In the aquatic products course of working, often have operation processes such as washing, centrifugation, filtration, and can contain a large amount of microorganisms and organic matter in the waste water that these processes produced, according to the requirement of country to environmental protection and sustainable development, the waste water that the aquatic products course of working produced need carry out germicidal treatment just can discharge, compares with traditional organic antibacterial agent, and nano-material's specific surface area is high, reactive activity is high, can effectively improve antibacterial effect.
The nano silver has an excellent antibacterial effect, but the pure nano silver is easy to agglomerate when being put into sewage, the dispersibility is very poor, so that the antibacterial effect is poor, the epoxy resin has the advantages of good mechanical property, electrical insulation, low shrinkage rate, high temperature resistance, stable chemical property and the like, but the epoxy resin has poor thermal stability, poor ageing resistance and no antibacterial property, and the epoxy resin needs to be subjected to chemical modification treatment to endow the epoxy resin with good thermal stability, ageing resistance and antibacterial property, so that the problem is solved by adopting a mode of doping the modified nano Ag with the epoxy resin.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the modified nano Ag-doped epoxy resin antibacterial material and the preparation method thereof, and solves the problems of poor thermal stability, poor aging resistance and no antibacterial property of the epoxy resin.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the modified nano Ag-doped epoxy resin antibacterial material comprises the following steps:
(1) adding Tris buffer solution and dopamine into a beaker, adding dilute hydrochloric acid to adjust the pH value of the solution to 8.0, placing the solution in a magnetic stirrer, stirring for 12-24 hours, centrifuging, washing and drying to obtain polydopamine nanoparticles;
(2) adding deionized water, silver nitrate and polydopamine nanoparticles into a beaker, adjusting the pH value of the solution to 9-12, performing ultrasonic treatment for 3-5 hours to uniformly disperse, filtering, washing and drying to obtain nano Ag-doped polydopamine nanoparticles;
(3) adding deionized water and sodium hexametaphosphate into a beaker, performing ultrasonic treatment for 30-90min to disperse uniformly, adding nano Ag doped polydopamine nano-particles and polyethyleneimine, magnetically stirring at room temperature for 12-36h, centrifuging, washing and drying to obtain high-molecular functionalized nano Ag doped polydopamine nano-particles;
(4) adding ethanol and polymer functionalized nano Ag doped polydopamine nanoparticles into a beaker, performing ultrasonic treatment for 1-3h to disperse uniformly, adding epoxy resin preheated to 70-90 ℃, stirring vigorously to mix uniformly, then placing the beaker in an oven at 80-100 ℃ for 6-18h to remove a solvent, heating the obtained product to 60-80 ℃, adding a curing agent diethylenetriamine, stirring vigorously to mix uniformly, placing the mixture in a mould for vacuum degassing for 1-3h at 60-80 ℃, placing the obtained mixed solution in the mould, curing for 12-24h at 70-90 ℃, and then curing for 3-5h at 150-170 ℃ to obtain the modified nano Ag doped epoxy resin antibacterial material.
Preferably, the magnetic stirrer in the step (1) comprises a main body, a motor is movably connected to the bottom of the main body, a fixing plate is movably connected to the bottom of the main body, a first gear is movably connected to the middle of the fixing plate, a second gear is movably connected to the left side of the first gear, a third gear is movably connected to the left side of the second gear, a fourth gear is movably connected to the left side of the third gear, a south-pole magnetic sheet is movably connected to the bottom of the second gear, a north-pole magnetic sheet is movably connected to the bottom of the fourth gear, a bottom plate is movably connected to the middle of the main body.
Preferably, the mass ratio of the silver nitrate to the polydopamine nanoparticles in the step (2) is 100: 10-20.
Preferably, the mass ratio of the sodium hexametaphosphate to the nano Ag doped polydopamine nanoparticles to the polyethyleneimine in the step (3) is 10-16:100: 90-110.
Preferably, the mass ratio of the polymer functionalized nano Ag doped poly dopamine nanoparticles, the epoxy resin and the diethylenetriamine in the step (4) is 100:0.5-4: 10-16.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the modified nano Ag-doped epoxy resin antibacterial material has the advantages that polydopamine nanoparticles contain rich phenolic hydroxyl groups, can capture free radical groups which cause material degradation and aging due to ultraviolet irradiation, reduce the decomposition effect of the free radicals on the antibacterial material, delay the ultraviolet degradation process of the antibacterial material, and obtain nano Ag-doped polydopamine nanoparticles by taking silver nitrate as a silver source and performing ultrasonic treatment, wherein the polydopamine nanoparticles contain rich phenolic hydroxyl groups and quinone groups, can chelate silver ions, reduce the silver ions into nano simple substance silver, combine the nano silver with cell membranes and cell wall DNA, replace hydrogen bonds between thymine and cytosine guanine in a DNA double-helix structure, cause the deformation of a bacterial DNA molecular structure, inhibit the synthesis of DNA, RNA and protein, are bacteria and are inactivated, and meanwhile, the nano silver has higher catalytic capacity due to the unique chemical structure, the reduction potential of the high titanium oxide silver is extremely high, the high titanium oxide silver is enough to generate atomic oxygen in the surrounding space, the high titanium oxide silver has strong oxidizing property and can be effectively sterilized, in addition, the silver has the specific surface plasmon resonance effect of noble metal, so that photons in visible light irradiation can be absorbed by the nano silver to generate photoproduction electrons and holes, the surface plasmon resonance effect leads to the enhancement of the magnetic field in the silver, the separation of the photoproduction electrons and the holes is promoted, and the photocatalytic antibacterial activity of the material is improved.
According to the modified nano Ag-doped epoxy resin antibacterial material, under the action of sodium hexametaphosphate, polyethyleneimine reacts with nano Ag-doped polydopamine nanoparticles to obtain high-molecular functionalized nano Ag-doped polydopamine nanoparticles, a large number of amino groups are introduced to the surface of the high-molecular functionalized nano Ag-doped polydopamine nanoparticles and perform a cross-linking reaction with epoxy resin, the dispersibility and compatibility of the high-molecular functionalized nano Ag-doped polydopamine nanoparticles in the epoxy resin are improved, the epoxy resin is endowed with excellent antibacterial performance and ageing resistance, meanwhile, chemical bonds formed by the cross-linking reaction reduce the free volume of the composite material, the cross-linking density is improved, the high-molecular functionalized nano Ag-doped polydopamine nanoparticles limit the movement chain segments of the epoxy resin, and the thermal stability of the composite material is improved.
Drawings
FIG. 1 is a front sectional structural schematic view of a magnetic stirrer;
fig. 2 is a schematic view of a gear transmission structure.
1. A main body; 2. a motor; 3. a fixing plate; 4. a first gear; 5. a second gear; 6. a third gear; 7. a fourth gear; 8. a magnetic sheet for south pole; 9. a north pole magnetic sheet; 10. a base plate; 11. and (4) a beaker.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: the preparation method of the modified nano Ag-doped epoxy resin antibacterial material comprises the following steps:
(1) adding Tris buffer solution and dopamine into a beaker, adding dilute hydrochloric acid to adjust the pH value of the solution to 8.0, and placing the beaker into a magnetic stirrer, wherein the magnetic stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the bottom of the main body is movably connected with a fixed plate, the middle of the fixed plate is movably connected with a first gear, the left side of the first gear is movably connected with a second gear, the left side of the second gear is movably connected with a third gear, the left side of the third gear is movably connected with a fourth gear, the bottom of the second gear is movably connected with a south pole magnetic sheet, the bottom of the fourth gear is movably connected with a north pole magnetic sheet, the middle of the main body is movably connected with a bottom plate, the top of the bottom plate is movably connected with the beaker;
(2) adding deionized water, silver nitrate and polydopamine nanoparticles into a beaker in a mass ratio of 100:10-20, adjusting the pH of the solution to 9-12, performing ultrasonic treatment for 3-5 hours to uniformly disperse, filtering, washing and drying to obtain nano Ag-doped polydopamine nanoparticles;
(3) adding deionized water and sodium hexametaphosphate into a beaker, performing ultrasonic treatment for 30-90min to disperse uniformly, adding nano Ag-doped polydopamine nanoparticles and polyethyleneimine, wherein the mass ratio of the sodium hexametaphosphate to the nano Ag-doped polydopamine nanoparticles to the polyethyleneimine is 10-16:100:90-110, magnetically stirring at room temperature for 12-36h, centrifuging, washing and drying to obtain high-molecular functionalized nano Ag-doped polydopamine nanoparticles;
(4) adding ethanol and polymer functionalized nano Ag doped polydopamine nanoparticles into a beaker, performing ultrasonic treatment for 1-3h to disperse uniformly, adding epoxy resin preheated to 70-90 ℃, stirring vigorously to mix the mixture uniformly, then placing the mixture in an oven at 80-100 ℃ for treatment for 6-18h to remove a solvent, heating the obtained product to 60-80 ℃, adding a curing agent diethylenetriamine, wherein the mass ratio of the polymer functionalized nano Ag doped polydopamine nanoparticles to the epoxy resin to the diethylenetriamine is 100:0.5-4:10-16, stirring vigorously to mix the mixture uniformly, then placing the mixture in a mould for vacuum degassing for 1-3h at 60-80 ℃, placing the obtained mixed solution in the mould, curing the mixed solution for 12-24h at 70-90 ℃, and then curing the mixed solution for 3-5h at 150 ℃ and 170 ℃, obtaining the modified nano Ag-doped epoxy resin antibacterial material.
Example 1
(1) Adding Tris buffer solution and dopamine into a beaker, adding dilute hydrochloric acid to adjust the pH value of the solution to 8.0, and placing the beaker into a magnetic stirrer, wherein the magnetic stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the bottom of the main body is movably connected with a fixed plate, the middle of the fixed plate is movably connected with a first gear, the left side of the first gear is movably connected with a second gear, the left side of the second gear is movably connected with a third gear, the left side of the third gear is movably connected with a fourth gear, the bottom of the second gear is movably connected with a south pole magnetic sheet, the bottom of the fourth gear is movably connected with a north pole magnetic sheet, the middle of the main body is movably connected with a bottom plate, the top of the bottom plate is movably connected with the;
(2) adding deionized water, silver nitrate and polydopamine nanoparticles into a beaker, wherein the mass ratio of the deionized water to the silver nitrate to the polydopamine nanoparticles is 100:10, adjusting the pH value of the solution to be 9, carrying out ultrasonic treatment for 3 hours to uniformly disperse the solution, and filtering, washing and drying the solution to obtain nano Ag-doped polydopamine nanoparticles;
(3) adding deionized water and sodium hexametaphosphate into a beaker, performing ultrasonic treatment for 30min to disperse uniformly, adding nano Ag doped polydopamine nanoparticles and polyethyleneimine, wherein the mass ratio of the sodium hexametaphosphate to the nano Ag doped polydopamine nanoparticles to the polyethyleneimine is 10:100:90, magnetically stirring at room temperature for 12h, centrifuging, washing and drying to obtain high-molecular functionalized nano Ag doped polydopamine nanoparticles;
(4) adding ethanol and polymer functionalized nano Ag doped polydopamine nanoparticles into a beaker, carrying out ultrasonic treatment for 1 hour to disperse uniformly, adding epoxy resin preheated to 70 ℃, carrying out vigorous stirring to mix uniformly, then placing the beaker in an oven at 80 ℃ for 6 hours to remove the solvent, heating the obtained product to 60 ℃, adding a curing agent diethylenetriamine, wherein the mass ratio of the polymer functionalized nano Ag doped polydopamine nanoparticles to the epoxy resin to the diethylenetriamine is 100:0.5:10, carrying out vigorous stirring to mix uniformly, then placing the mixture in a mold for vacuum degassing for 1 hour at 60 ℃, placing the obtained mixture in a mold, curing the mixture at 70 ℃ for 12 hours, and then curing the mixture at 150 ℃ for 3 hours to obtain the modified nano Ag doped epoxy resin antibacterial material.
Example 2
(1) Adding Tris buffer solution and dopamine into a beaker, adding dilute hydrochloric acid to adjust the pH value of the solution to 8.0, and placing the beaker into a magnetic stirrer, wherein the magnetic stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the bottom of the main body is movably connected with a fixed plate, the middle of the fixed plate is movably connected with a first gear, the left side of the first gear is movably connected with a second gear, the left side of the second gear is movably connected with a third gear, the left side of the third gear is movably connected with a fourth gear, the bottom of the second gear is movably connected with a south pole magnetic sheet, the bottom of the fourth gear is movably connected with a north pole magnetic sheet, the middle of the main body is movably connected with a bottom plate, the top of the bottom plate is movably connected with the;
(2) adding deionized water, silver nitrate and polydopamine nanoparticles into a beaker in a mass ratio of 100:13, adjusting the pH value of the solution to 10, carrying out ultrasonic treatment for 3 hours to uniformly disperse the solution, filtering, washing and drying the solution to obtain nano Ag-doped polydopamine nanoparticles;
(3) adding deionized water and sodium hexametaphosphate into a beaker, performing ultrasonic treatment for 50min to disperse uniformly, adding nano Ag doped polydopamine nanoparticles and polyethyleneimine, wherein the mass ratio of the sodium hexametaphosphate to the nano Ag doped polydopamine nanoparticles to the polyethyleneimine is 14:100:98, magnetically stirring for 20h at room temperature, centrifuging, washing and drying to obtain high-molecular functionalized nano Ag doped polydopamine nanoparticles;
(4) adding ethanol and polymer functionalized nano Ag doped polydopamine nanoparticles into a beaker, performing ultrasonic treatment for 1 hour to disperse uniformly, adding epoxy resin preheated to 75 ℃, stirring vigorously to mix uniformly, then placing the beaker in an oven at 85 ℃ for 10 hours to remove a solvent, heating the obtained product to 65 ℃, adding a curing agent diethylenetriamine, wherein the mass ratio of the polymer functionalized nano Ag doped polydopamine nanoparticles to the epoxy resin to the diethylenetriamine is 100:1:12, stirring vigorously to mix uniformly, then placing the mixture in a vacuum at 65 ℃ for degassing for 3 hours, placing the obtained mixed solution in a mold, curing the mixture at 75 ℃ for 15 hours, and then curing the mixture at 155 ℃ for 3 hours to obtain the modified nano Ag doped epoxy resin antibacterial material.
Example 3
(1) Adding Tris buffer solution and dopamine into a beaker, adding dilute hydrochloric acid to adjust the pH value of the solution to 8.0, and placing the beaker into a magnetic stirrer, wherein the magnetic stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the bottom of the main body is movably connected with a fixed plate, the middle of the fixed plate is movably connected with a first gear, the left side of the first gear is movably connected with a second gear, the left side of the second gear is movably connected with a third gear, the left side of the third gear is movably connected with a fourth gear, the bottom of the second gear is movably connected with a south pole magnetic sheet, the bottom of the fourth gear is movably connected with a north pole magnetic sheet, the middle of the main body is movably connected with a bottom plate, the top of the bottom plate is movably connected with the;
(2) adding deionized water, silver nitrate and polydopamine nanoparticles into a beaker at a mass ratio of 100:15, adjusting the pH of the solution to 10.5, ultrasonically dispersing the solution for 4 hours uniformly, filtering, washing and drying the solution to obtain nano Ag-doped polydopamine nanoparticles;
(3) adding deionized water and sodium hexametaphosphate into a beaker, performing ultrasonic treatment for 60min to disperse uniformly, adding nano Ag doped polydopamine nanoparticles and polyethyleneimine, wherein the mass ratio of the sodium hexametaphosphate to the nano Ag doped polydopamine nanoparticles to the polyethyleneimine is 13:100:100, magnetically stirring at room temperature for 18h, centrifuging, washing and drying to obtain high-molecular functionalized nano Ag doped polydopamine nanoparticles;
(4) adding ethanol and polymer functionalized nano Ag doped polydopamine nanoparticles into a beaker, carrying out ultrasonic treatment for 2h to disperse uniformly, adding epoxy resin preheated to 80 ℃, carrying out vigorous stirring to mix uniformly, then placing the beaker in an oven at 90 ℃ for 12h to remove the solvent, heating the obtained product to 70 ℃, adding a curing agent diethylenetriamine, wherein the mass ratio of the polymer functionalized nano Ag doped polydopamine nanoparticles to the epoxy resin to the diethylenetriamine is 100:2.5:13, carrying out vigorous stirring to mix uniformly, then placing the mixture in a vacuum degassing chamber at 70 ℃ for 2h, placing the obtained mixed solution in a mold, curing the mixture at 80 ℃ for 18h, and then curing the mixture at 16 ℃ for 4h to obtain the modified nano Ag doped epoxy resin antibacterial material.
Example 4
(1) Adding Tris buffer solution and dopamine into a beaker, adding dilute hydrochloric acid to adjust the pH value of the solution to 8.0, and placing the beaker into a magnetic stirrer, wherein the magnetic stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the bottom of the main body is movably connected with a fixed plate, the middle of the fixed plate is movably connected with a first gear, the left side of the first gear is movably connected with a second gear, the left side of the second gear is movably connected with a third gear, the left side of the third gear is movably connected with a fourth gear, the bottom of the second gear is movably connected with a south pole magnetic sheet, the bottom of the fourth gear is movably connected with a north pole magnetic sheet, the middle of the main body is movably connected with a bottom plate, the top of the bottom plate is movably connected with the;
(2) adding deionized water, silver nitrate and polydopamine nanoparticles into a beaker in a mass ratio of 100:20, adjusting the pH of the solution to be 12, ultrasonically dispersing the solution uniformly for 5 hours, filtering, washing and drying the solution to obtain nano Ag-doped polydopamine nanoparticles;
(3) adding deionized water and sodium hexametaphosphate into a beaker, performing ultrasonic treatment for 90min to disperse uniformly, adding nano Ag doped polydopamine nanoparticles and polyethyleneimine, wherein the mass ratio of the sodium hexametaphosphate to the nano Ag doped polydopamine nanoparticles to the polyethyleneimine is 16:100:110, magnetically stirring for 36h at room temperature, centrifuging, washing and drying to obtain high-molecular functionalized nano Ag doped polydopamine nanoparticles;
(4) adding ethanol and polymer functionalized nano Ag doped polydopamine nanoparticles into a beaker, carrying out ultrasonic treatment for 3h to disperse uniformly, adding epoxy resin preheated to 90 ℃, carrying out vigorous stirring to mix uniformly, then placing the beaker in an oven at 100 ℃ for 18h to remove the solvent, heating the obtained product to 80 ℃, adding a curing agent diethylenetriamine, wherein the mass ratio of the polymer functionalized nano Ag doped polydopamine nanoparticles to the epoxy resin to the diethylenetriamine is 100:4:16, carrying out vigorous stirring to mix uniformly, then placing the mixture in a vacuum degassing chamber at 80 ℃ for 3h, placing the obtained mixed solution in a mold, curing the mixed solution at 90 ℃ for 24h, and then curing the mixed solution at 170 ℃ for 5h to obtain the modified nano Ag doped epoxy resin antibacterial material.
Comparative example 1
(1) Adding Tris buffer solution and dopamine into a beaker, adding dilute hydrochloric acid to adjust the pH value of the solution to 8.0, and placing the beaker into a magnetic stirrer, wherein the magnetic stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the bottom of the main body is movably connected with a fixed plate, the middle of the fixed plate is movably connected with a first gear, the left side of the first gear is movably connected with a second gear, the left side of the second gear is movably connected with a third gear, the left side of the third gear is movably connected with a fourth gear, the bottom of the second gear is movably connected with a south pole magnetic sheet, the bottom of the fourth gear is movably connected with a north pole magnetic sheet, the middle of the main body is movably connected with a bottom plate, the top of the bottom plate is movably connected with the;
(2) adding deionized water, silver nitrate and polydopamine nanoparticles into a beaker in a mass ratio of 100:8, adjusting the pH of the solution to 9, ultrasonically dispersing the solution uniformly for 5 hours, filtering, washing and drying the solution to obtain nano Ag-doped polydopamine nanoparticles;
(3) adding deionized water and sodium hexametaphosphate into a beaker, performing ultrasonic treatment for 40min to disperse uniformly, adding nano Ag doped polydopamine nanoparticles and polyethyleneimine, wherein the mass ratio of the sodium hexametaphosphate to the nano Ag doped polydopamine nanoparticles to the polyethyleneimine is 8:100:80, magnetically stirring for 24h at room temperature, centrifuging, washing and drying to obtain high-molecular functionalized nano Ag doped polydopamine nanoparticles;
(4) adding ethanol and polymer functionalized nano Ag doped polydopamine nanoparticles into a beaker, carrying out ultrasonic treatment for 1 hour to disperse uniformly, adding epoxy resin preheated to 70 ℃, carrying out vigorous stirring to mix uniformly, then placing the beaker in an oven at 100 ℃ for 6 hours to remove the solvent, heating the obtained product to 80 ℃, adding a curing agent diethylenetriamine, wherein the mass ratio of the polymer functionalized nano Ag doped polydopamine nanoparticles to the epoxy resin to the diethylenetriamine is 100:5:8, carrying out vigorous stirring to mix uniformly, then placing the mixture in a vacuum degassing chamber at 70 ℃ for 1 hour, placing the obtained mixed solution in a mold, curing the mixed solution at 80 ℃ for 12 hours, and then curing the mixed solution at 155 ℃ for 3 hours to obtain the modified nano Ag doped epoxy resin antibacterial material.
The modified nano Ag-doped epoxy resin antibacterial materials obtained in the examples and comparative examples were irradiated with ultraviolet for 60min, 100ul was diluted to 106Inoculating CFU/ml test bacterial liquid on the front surface of the sample membrane irradiated by ultraviolet, culturing at constant temperature for 12h, eluting bacteria on the surface of the sample membrane with physiological saline, and adding the eluted bacteria at a ratio of 1:106Diluting with normal saline, culturing with appropriate amount of bacterial liquid and solid culture medium, observing with microscope, calculating concentration, and calculating antibacterial rate with GB/T21866-.
Claims (5)
1. A modified nano Ag-doped epoxy resin antibacterial material is characterized in that: the preparation method of the modified nano Ag-doped epoxy resin antibacterial material comprises the following steps:
(1) adding Tris buffer solution and dopamine into a beaker, adding dilute hydrochloric acid to adjust the pH value of the solution to 8.0, placing the solution in a magnetic stirrer, stirring for 12-24 hours, centrifuging, washing and drying to obtain polydopamine nanoparticles;
(2) adding deionized water, silver nitrate and polydopamine nanoparticles into a beaker, adjusting the pH value of the solution to 9-12, performing ultrasonic treatment for 3-5 hours to uniformly disperse, filtering, washing and drying to obtain nano Ag-doped polydopamine nanoparticles;
(3) adding deionized water and sodium hexametaphosphate into a beaker, performing ultrasonic treatment for 30-90min to disperse uniformly, adding nano Ag doped polydopamine nano-particles and polyethyleneimine, magnetically stirring at room temperature for 12-36h, centrifuging, washing and drying to obtain high-molecular functionalized nano Ag doped polydopamine nano-particles;
(4) adding ethanol and polymer functionalized nano Ag doped polydopamine nanoparticles into a beaker, performing ultrasonic treatment for 1-3h to disperse uniformly, adding epoxy resin preheated to 70-90 ℃, stirring vigorously to mix uniformly, then placing the beaker in an oven at 80-100 ℃ for 6-18h to remove a solvent, heating the obtained product to 60-80 ℃, adding a curing agent diethylenetriamine, stirring vigorously to mix uniformly, placing the mixture in a mould for vacuum degassing for 1-3h at 60-80 ℃, placing the obtained mixed solution in the mould, curing for 12-24h at 70-90 ℃, and then curing for 3-5h at 150-170 ℃ to obtain the modified nano Ag doped epoxy resin antibacterial material.
2. The modified nano Ag-doped epoxy resin antibacterial material according to claim 1, which is characterized in that: the magnetic stirrer in the step (1) comprises a main body, a motor is movably connected to the bottom of the main body, a fixing plate is movably connected to the bottom of the main body, a first gear is movably connected to the middle of the fixing plate, a second gear is movably connected to the left side of the first gear, a third gear is movably connected to the left side of the second gear, a fourth gear is movably connected to the left side of the third gear, a south pole magnetic sheet is movably connected to the bottom of the second gear, a north pole magnetic sheet is movably connected to the bottom of the fourth gear, a bottom plate is movably connected to the middle of the main body, and.
3. The modified nano Ag-doped epoxy resin antibacterial material according to claim 1, which is characterized in that: the mass ratio of the silver nitrate to the polydopamine nanoparticles in the step (2) is 100: 10-20.
4. The modified nano Ag-doped epoxy resin antibacterial material according to claim 1, which is characterized in that: in the step (3), the mass ratio of the sodium hexametaphosphate to the nano Ag-doped polydopamine nano-particles to the polyethyleneimine is 10-16:100: 90-110.
5. The modified nano Ag-doped epoxy resin antibacterial material according to claim 1, which is characterized in that: the mass ratio of the polymer functionalized nano Ag doped polydopamine nano particles, the epoxy resin and the diethylenetriamine in the step (4) is 100:0.5-4: 10-16.
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Application publication date: 20200825 |