CN112616853A - Preparation method of high-dispersion anti-discoloration nano-silver antibacterial agent material - Google Patents
Preparation method of high-dispersion anti-discoloration nano-silver antibacterial agent material Download PDFInfo
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- CN112616853A CN112616853A CN202011454764.XA CN202011454764A CN112616853A CN 112616853 A CN112616853 A CN 112616853A CN 202011454764 A CN202011454764 A CN 202011454764A CN 112616853 A CN112616853 A CN 112616853A
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention relates to a preparation method of a high-dispersion anti-discoloration nano-silver antibacterial agent material, belonging to the technical field of antibacterial materials. According to the technical scheme, porous titanium dioxide particles are prepared as a load base material of the material, the base material has an excellent pore structure, the arrangement of inner pore channels is basically disordered, pore walls are amorphous, one-dimensional pore channels are intersected with each other to form a vermicular pore channel structure in three-dimensional cross arrangement, and the diffusion of load material molecules in the pore channels is facilitated.
Description
Technical Field
The invention relates to a preparation method of a high-dispersion anti-discoloration nano-silver antibacterial agent material, belonging to the technical field of antibacterial materials.
Background
The silver ions react with the bacteria to cause the destruction or dysfunction of the inherent components of the bacteria, thereby causing the death of the bacteria. Because the cell membrane of the microorganism is always provided with negative charges, silver ions can be firmly adsorbed on the cell membrane by means of coulomb attraction, and can further penetrate through the cell wall to enter the bacteria and react with sulfydryl in the bacteria, so that the protein of the bacteria is solidified, the activity of cell synthase of the bacteria is damaged, the cells lose division and proliferation capacity and die, and meanwhile, the silver ions can also damage an electron transmission system, a respiratory system and a substance transmission system of the microorganism. When the thallus loses activity, silver ions are dissociated from the thallus, and the sterilization activity is repeated, so that the antibacterial effect is durable.
However, the existing silver nano material is sensitive to light due to the silver-containing component, and is easy to generate color change under illumination, and the silver-containing nano material is also easy to react with sulfur, phosphorus and the like in the additive to change color after being added into an antibacterial product. The discoloration problem seriously affects the appearance properties of the antimicrobial article. Meanwhile, due to poor dispersion performance of the nano-silver, the material is dispersed unevenly, and is easy to agglomerate to reduce the overall performance of the material, so that modification of the nano-silver is necessary.
Disclosure of Invention
The invention aims to provide a preparation method of a high-dispersion anti-discoloration nano-silver antibacterial agent material, which aims to solve one of the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the preparation method of the high-dispersion anti-tarnishing nano-silver antibacterial material comprises the following specific preparation steps:
s1, mixing isooctane, lecithin and titanium isopropoxide serving as raw materials, collecting gel liquid, and calcining at high temperature to prepare matrix particles; s2, drying the matrix particles, and modifying the matrix particles by using deionized water, hydrochloric acid, epichlorohydrin and sodium carboxymethylcellulose to prepare modified matrix particles; s3, preparing a mixed sol solution by using deionized water, cetyl trimethyl ammonium bromide, a silver nitrate solution, hydrazine hydrate and a silver nitrate solution, loading the silver nitrate solution on the mixed sol solution to prepare a base body fluid, and preparing the mixed sol solution by placing the base body fluid, TEOS, ammonia water and absolute ethyl alcohol; and S4, mixing the mixed sol solution with the modified matrix particles, drying and curing to prepare the high-dispersion anti-discoloration nano-silver antibacterial material.
The mixing proportion of the isooctane, the lecithin and the titanium isopropoxide prepared in the step S1 is that 45-50 parts by weight of isooctane, 6-8 parts by weight of lecithin and 3-5 parts by weight of titanium isopropoxide are respectively weighed.
And the high-temperature calcination treatment in the step S1 is to take the gel liquid, place the gel liquid in a muffle furnace, heat the gel liquid to 400-500 ℃ at a speed of 5 ℃/min, perform heat preservation reaction, heat the gel liquid to 520-550 ℃ at a speed of 2 ℃/min, and perform heat preservation reaction for 3-5 hours. The porous titanium dioxide particles are prepared as the loading matrix material of the material, the matrix material has an excellent pore structure, the arrangement of the inner pore channels is basically disordered, the pore wall composition is amorphous, but one-dimensional pore channels are crossed with each other to form a three-dimensional cross-arranged vermicular pore channel structure, so that the diffusion of the loaded material molecules in the pore channels is facilitated, and the material has excellent loading performance firstly when being used as the material loading matrix.
The specific modification step of step S2 is: s21, taking and drying the matrix particles to prepare dry matrix particles, respectively weighing 45-50 parts by weight of deionized water, 1-2 parts by weight of 1% hydrochloric acid, 45-50 parts by weight of epoxy chloropropane and 10-15 parts by weight of dry matrix particles, placing the mixture in a beaker, stirring and mixing the mixture, adjusting the pH value to 7.0 by using 10% sodium hydroxide, stirring and mixing the mixture, and collecting a mixed solution; s22, adding sodium carboxymethylcellulose into the mixed solution according to the mass ratio of 1:15, performing ultrasonic dispersion for 10-15 min at 200-300W, performing heat preservation reaction for 5-8 h at 45-55 ℃, filtering, collecting lower-layer precipitates, and drying for 6-8 h to prepare modified matrix particles; the OH-groups contained in the sodium carboxymethyl cellulose material are loaded to the inside of the pore channel of the material, so that the sodium carboxymethyl cellulose material is solidified and coats the inside of the pore channel, the firmness of the pore channel structure of the material is improved, the adsorption capacity of the material is improved, and the adsorption performance of the material is further improved.
The mixing proportion of the deionized water, the hexadecyl trimethyl ammonium bromide, the silver nitrate solution, the hydrazine hydrate and the silver nitrate solution in the step S3 is as follows: according to the weight parts, 45-50 parts of deionized water, 3-5 parts of hexadecyl trimethyl ammonium bromide, 6-8 parts of silver nitrate solution with the mass fraction of 5% and 6-8 parts of hydrazine hydrate are respectively weighed. The composite sol system is prepared by compounding silver nitrate and nano-silica sol, the number of the loaded silver ions can be effectively improved in the porous matrix material with the effective load value of the system, so that the antibacterial property of the material is more excellent, and meanwhile, the material is effectively loaded and coated in pores of the material, so that the solidified loaded nano-antibacterial material has more excellent antibacterial property, and the antibacterial property of the material is effectively improved.
The preparation step of the mixed sol solution in the step S3 is as follows: respectively weighing 45-50 parts by weight of base fluid, 10-15 parts by weight of TEOS, 3-5 parts by weight of 10% ammonia water and 25-30 parts by weight of absolute ethyl alcohol, placing the mixture in a beaker, stirring, mixing, standing for 6-8 hours, and collecting to obtain a mixed sol solution.
The drying and curing temperature of the step S4 is 100-110 ℃.
Compared with the prior art, the invention has the beneficial effects that: (1) according to the technical scheme, porous titanium dioxide particles are prepared as a load matrix material of the material, the matrix material has an excellent pore structure, the arrangement of inner pore channels is basically disordered, pore walls are amorphous, one-dimensional pore channels are intersected with each other to form a worm-shaped pore channel structure in three-dimensional cross arrangement, and the diffusion of load material molecules in the pore channels is facilitated;
(2) according to the technical scheme, OH-groups contained in the carboxymethylcellulose sodium material are loaded into the pore channels of the material, so that the carboxymethylcellulose sodium material is solidified and coats the interior of the pore channels, the firmness of the pore channel structure of the material is improved, the adsorption capacity of the material is improved, and the adsorption performance of the material is further improved;
(3) according to the technical scheme, the silver nitrate and the nano-silica sol are compounded to prepare the composite sol system, the number of the loaded silver ions can be effectively improved in the porous matrix material of the system effective load value, so that the antibacterial performance of the composite sol system is more excellent, meanwhile, the material is effectively loaded and coated in the pores of the material, and the solidified loaded nano-antibacterial material has more excellent antibacterial performance, so that the antibacterial performance of the material is effectively improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Respectively weighing 45-50 parts by weight of isooctane, 6-8 parts by weight of lecithin and 3-5 parts by weight of titanium isopropoxide, placing the materials into a three-neck flask, stirring and mixing the materials, placing the materials into a 200-300W ultrasonic dispersion machine for 10-15 min, collecting dispersion gel, stirring and mixing the dispersion gel and deionized water according to the mass ratio of 1:5, collecting mixed slurry, placing the mixed slurry into a 55-60 ℃ drying machine for 20-24 h, collecting dried substances, placing the dried substances into a muffle furnace, heating to 400-500 ℃ according to 5 ℃/min, carrying out heat preservation reaction, heating to 520-550 ℃ according to 2 ℃/min, carrying out heat preservation reaction for 3-5 h, standing and cooling to room temperature, grinding the materials to pass through a 200-mesh sieve, and collecting matrix particles; taking matrix particles, washing the matrix particles with deionized water, drying the matrix particles at 100-110 ℃ for 20-24 h, and collecting the dried matrix particles; respectively weighing 45-50 parts by weight of deionized water, 1-2 parts by weight of 1% hydrochloric acid, 45-50 parts by weight of epichlorohydrin and 10-15 parts by weight of dry matrix particles, placing the materials into a beaker, stirring and mixing the materials, adjusting the pH to 7.0 by using 10% sodium hydroxide, stirring and mixing the materials, collecting a mixed solution, adding sodium carboxymethylcellulose into the mixed solution according to the mass ratio of 1:15, performing ultrasonic dispersion at 200-300W for 10-15 min, performing heat preservation reaction at 45-55 ℃ for 5-8 h, filtering and collecting lower-layer precipitates, and drying the lower-layer precipitates for 6-8 h to prepare modified matrix particles; respectively weighing 45-50 parts by weight of deionized water, 3-5 parts by weight of hexadecyl trimethyl ammonium bromide, 6-8 parts by weight of 5% silver nitrate solution and 6-8 parts by weight of hydrazine hydrate, stirring and mixing, collecting mixed reaction liquid, dropwise adding the silver nitrate solution with the mass fraction of 2% into the mixed reaction liquid according to the mass ratio of 1:15, controlling the dropwise adding speed to be 2-3 mL/min, and stirring, mixing and collecting to obtain base body liquid after dropwise adding is completed; respectively weighing 45-50 parts by weight of base fluid, 10-15 parts by weight of TEOS, 3-5 parts by weight of 10% ammonia water and 25-30 parts by weight of absolute ethyl alcohol, placing the mixture in a beaker, stirring, mixing and standing for 6-8 hours, collecting to obtain a mixed sol solution, adding dry base particles into the mixed sol solution according to the mass ratio of 1:10, standing for 3-5 hours, performing ultrasonic dispersion and filtration, collecting a filter cake, placing the filter cake at 100-110 ℃ for drying to constant weight, and collecting dry particles to obtain the high-dispersion anti-discoloration nano silver antibacterial agent material.
Example 1
Respectively weighing 45 parts by weight of isooctane, 6 parts by weight of lecithin and 3 parts by weight of titanium isopropoxide, placing the materials into a three-neck flask, stirring and mixing the materials, placing the materials into a 200W ultrasonic stirrer for 10min, collecting dispersion gel, stirring and mixing the dispersion gel with deionized water according to the mass ratio of 1:5, collecting mixed slurry, placing the mixed slurry into a muffle furnace for drying at 55 ℃ for 20h, collecting the dried product, placing the dried product into the muffle furnace, heating to 400 ℃ at the speed of 5 ℃/min, carrying out heat preservation reaction, heating to 520 ℃ at the speed of 2 ℃/min, carrying out heat preservation reaction for 3h, standing, cooling to room temperature, grinding the product to 200 meshes, and collecting matrix particles; taking matrix particles, washing the matrix particles by deionized water, drying the matrix particles at 100 ℃ for 20 hours, and collecting the dried matrix particles; respectively weighing 45 parts of deionized water, 1 part of hydrochloric acid with the mass fraction of 1%, 45 parts of epoxy chloropropane and 10 parts of dry matrix particles in parts by weight, placing the materials into a beaker, stirring and mixing the materials, adjusting the pH value to 7.0 by using sodium hydroxide with the mass fraction of 10%, stirring and mixing the materials, collecting a mixed solution, adding sodium carboxymethyl cellulose into the mixed solution according to the mass ratio of 1:15, performing ultrasonic dispersion at 200W for 10min, performing heat preservation reaction at 45 ℃ for 5 hours, filtering and collecting lower-layer precipitates, and drying the lower-layer precipitates for 6-8 hours to prepare modified matrix particles; respectively weighing 45 parts of deionized water, 3 parts of hexadecyl trimethyl ammonium bromide, 6 parts of 5% silver nitrate solution in mass fraction and 6 parts of hydrazine hydrate, stirring and mixing, collecting mixed reaction liquid, dropwise adding the 2% silver nitrate solution in mass fraction into the mixed reaction liquid according to the mass ratio of 1:15, controlling the dropwise adding speed to be 2mL/min, and stirring, mixing and collecting to obtain base body liquid after dropwise adding is finished; respectively weighing 45 parts of base fluid, 10 parts of TEOS, 3 parts of 10% ammonia water and 25 parts of absolute ethyl alcohol in parts by weight, placing the mixture in a beaker, stirring, mixing and standing for 6 hours, collecting a mixed sol solution, adding dry matrix particles into the mixed sol solution according to the mass ratio of 1:10, standing for 3-5 hours, performing ultrasonic dispersion and filtration, collecting a filter cake, placing the filter cake at 100 ℃ for drying to constant weight, and collecting dry particles to obtain the high-dispersion anti-discoloration nano-silver antibacterial agent material.
Example 2
Respectively weighing 50 parts by weight of isooctane, 8 parts by weight of lecithin and 5 parts by weight of titanium isopropoxide, placing the materials into a three-neck flask, stirring and mixing the materials, placing the materials into a 300W ultrasonic dispersion machine for 15min, collecting dispersion gel, stirring and mixing the dispersion gel with deionized water according to the mass ratio of 1:5, collecting mixed slurry, placing the mixed slurry into a 60 ℃ drying machine for 24h, collecting dried substances, placing the dried substances into a muffle furnace, heating the dried substances to 500 ℃ according to the speed of 5 ℃/min, carrying out heat preservation reaction, heating the dried substances to 550 ℃ according to the speed of 2 ℃/min, carrying out heat preservation reaction for 5h, standing and cooling the dried substances to room temperature, grinding the cooled; taking matrix particles, washing the matrix particles by deionized water, drying the matrix particles at 110 ℃ for 24 hours, and collecting the dried matrix particles; respectively weighing 50 parts by weight of deionized water, 2 parts by weight of 1% hydrochloric acid, 50 parts by weight of epichlorohydrin and 10-15 parts by weight of dry matrix particles, placing the materials into a beaker, stirring and mixing the materials, adjusting the pH value to 7.0 by using 10% sodium hydroxide, stirring and mixing the materials, collecting a mixed solution, adding sodium carboxymethylcellulose into the mixed solution according to the mass ratio of 1:15, performing ultrasonic dispersion at 300W for 15min, performing heat preservation reaction at 55 ℃ for 8h, filtering and collecting lower-layer precipitates, and drying the lower-layer precipitates for 8h to prepare modified matrix particles; respectively weighing 50 parts by weight of deionized water, 5 parts by weight of hexadecyl trimethyl ammonium bromide, 8 parts by weight of 5% silver nitrate solution and 8 parts by weight of hydrazine hydrate, stirring and mixing, collecting mixed reaction liquid, dropwise adding the 2% silver nitrate solution into the mixed reaction liquid according to the mass ratio of 1:15, controlling the dropwise adding speed to be 3mL/min, and stirring, mixing and collecting to obtain base body liquid after the dropwise adding is finished; respectively weighing 50 parts by weight of base fluid, 15 parts by weight of TEOS, 5 parts by weight of 10% ammonia water and 30 parts by weight of absolute ethyl alcohol, placing the mixture in a beaker, stirring, mixing and standing for 8 hours, collecting mixed sol solution, adding dried matrix particles into the mixed sol solution according to the mass ratio of 1:10, standing for 5 hours, performing ultrasonic dispersion and filtration, collecting filter cakes, placing the filter cakes at 110 ℃ for drying to constant weight, and collecting dried particles to obtain the high-dispersion anti-discoloration nano-silver antibacterial agent material.
Example 3
Respectively weighing 47 parts by weight of isooctane, 7 parts by weight of lecithin and 4 parts by weight of titanium isopropoxide, placing the materials into a three-neck flask, stirring and mixing the materials, placing the materials into a 250W ultrasonic dispersion device for 12min, collecting dispersion gel, stirring and mixing the dispersion gel with deionized water according to the mass ratio of 1:5, collecting mixed slurry, placing the mixed slurry into a muffle furnace for drying at 57 ℃ for 22h, collecting the dried product, placing the dried product into the muffle furnace, heating to 450 ℃ at the speed of 5 ℃/min, carrying out heat preservation reaction, heating to 535 ℃ at the speed of 2 ℃/min, carrying out heat preservation reaction for 4h, standing, cooling to room temperature, grinding the product to pass through a 200-mesh; taking matrix particles, washing the matrix particles by deionized water, drying the matrix particles at 105 ℃ for 22 hours, and collecting the dried matrix particles; respectively weighing 47 parts by weight of deionized water, 1 part by weight of 1% hydrochloric acid, 47 parts by weight of epichlorohydrin and 12 parts by weight of dry matrix particles, placing the materials into a beaker, stirring and mixing the materials, adjusting the pH value to 7.0 by using 10% sodium hydroxide, stirring and mixing the materials, collecting a mixed solution, adding sodium carboxymethylcellulose into the mixed solution according to the mass ratio of 1:15, performing ultrasonic dispersion at 250W for 12min, performing heat preservation reaction at 47 ℃ for 7h, filtering and collecting lower-layer precipitates, and drying the lower-layer precipitates for 6-8 h to prepare modified matrix particles; respectively weighing 47 parts by weight of deionized water, 4 parts by weight of hexadecyl trimethyl ammonium bromide, 7 parts by weight of 5% silver nitrate solution and 7 parts by weight of hydrazine hydrate, stirring and mixing, collecting mixed reaction liquid, dropwise adding the 2% silver nitrate solution into the mixed reaction liquid according to the mass ratio of 1:15, controlling the dropwise adding speed to be 2mL/min, and stirring, mixing and collecting to obtain base body liquid after the dropwise adding is finished; respectively weighing 47 parts by weight of base fluid, 12 parts by weight of TEOS, 4 parts by weight of 10% ammonia water and 27 parts by weight of absolute ethyl alcohol, placing the mixture in a beaker, stirring, mixing and standing for 7 hours, collecting mixed sol solution, adding dried matrix particles into the mixed sol solution according to the mass ratio of 1:10, standing for 4 hours, performing ultrasonic dispersion and filtration, collecting filter cakes, placing the filter cakes at 105 ℃, drying to constant weight, collecting dried particles, and thus obtaining the high-dispersion anti-discoloration nano-silver antibacterial agent material.
Example 4
Respectively weighing 47 parts by weight of deionized water, 4 parts by weight of hexadecyl trimethyl ammonium bromide, 7 parts by weight of 5% silver nitrate solution and 7 parts by weight of hydrazine hydrate, stirring and mixing, collecting mixed reaction liquid, dropwise adding the 2% silver nitrate solution into the mixed reaction liquid according to the mass ratio of 1:15, controlling the dropwise adding speed to be 2mL/min, and stirring, mixing and collecting to obtain base body liquid after the dropwise adding is finished; respectively weighing 47 parts by weight of base fluid, 12 parts by weight of TEOS, 4 parts by weight of 10% ammonia water and 27 parts by weight of absolute ethyl alcohol, placing the mixture in a beaker, stirring, mixing and standing for 7 hours, collecting a mixed sol solution, adding zeolite into the mixed sol solution according to the mass ratio of 1:10, standing for 4 hours, performing ultrasonic dispersion and filtration, collecting a filter cake, placing the filter cake at 105 ℃, drying to constant weight, collecting dried particles, and thus obtaining the high-dispersion anti-discoloration nano-silver antibacterial agent material.
The antibacterial agent materials prepared in the invention, namely the embodiment 1, the embodiment 2, the embodiment 3 and the embodiment 4, are added into the resin PP, the addition amount of the antibacterial agent material is controlled to be 0.1%, the antibacterial resin is prepared by mixing, and then the antibacterial experiment is carried out according to the following steps:
1. sample pretreatment: tabletting the mixed resin to prepare an experimental slice with the thickness of 2mm, scrubbing the surface by using 75% ethanol solution, and placing the experimental slice into a dish with wet filter paper spread at the bottom for sterilization.
2. Preparing strains: and (3) carrying out shake culture on the bacterial suspension on a shaker at 37 ℃ for 24 hours, detecting the bacterial concentration, and diluting 100 mu l of bacterial suspension to 105-106 cuf/ml.
3. The diluted bacterial suspension is taken and coated on the surface of the resin, the weighing paper is covered on the surface, and the bacterial suspension is put into an incubator to be cultured for 24 hours at 37 ℃.
4. After the culture was completed, the surface of the resin was scrubbed with a sterile cotton ball, the weighing paper was crushed with forceps, 1ml of the supernatant was aspirated and placed in a petri dish, and after dilution ten times, the supernatant was cultured in an incubator at 37 ℃ for 24 hours.
5. Counting viable bacteria: and selecting a plate among 30-300 colonies as a colony total number determination standard. After counting the number of colonies on each plate, the average number of colonies on each plate of the same dilution was determined.
TABLE 1 comparison of Properties
As can be seen from the above table, examples 1, 2 and 3 prepared by the present invention have excellent antibacterial performance, and comparative example 4 has significantly reduced antibacterial performance and discoloration resistance compared with examples 1, 2 and 3, which illustrates that the technical solution of the present invention prepares porous titanium dioxide particles as a loading matrix material of a material, which is an effective photodegradation material, and at the same time, effectively absorbs ultraviolet rays, and has excellent improvement performance on discoloration resistance of the material, and at the same time, the technical solution of the present invention prepares a composite sol system by compounding silver nitrate and nano-silica sol, and the effective loading value of the system is inside the porous matrix material, on the basis of which, the amount of the loaded silver ions can be effectively improved, so that the antibacterial performance is more excellent, and the effective loading and coating of the material are inside the pores of the material, and the cured loaded nano-antibacterial material has more excellent antibacterial performance, thereby effectively improving the antibacterial property of the material.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (1)
1. A preparation method of a high-dispersion anti-tarnishing nano-silver antibacterial material is characterized by comprising the following steps: the preparation method comprises the following specific steps:
s1, respectively weighing 47 parts of isooctane, 7 parts of lecithin and 4 parts of titanium isopropoxide in parts by weight, placing the materials in a three-neck flask, stirring and mixing the materials, placing the materials in an ultrasonic dispersion device under 250W for 12min, collecting dispersion gel, stirring and mixing the dispersion gel and deionized water according to the mass ratio of 1:5, collecting mixed slurry, placing the mixed slurry in a muffle furnace for drying at 57 ℃ for 22h, collecting the dried product, placing the dried product in the muffle furnace, heating the dried product to 450 ℃ at 5 ℃/min, carrying out heat preservation reaction, heating the dried product to 535 ℃ at 2 ℃/min, carrying out heat preservation reaction for 4h, standing, cooling to room temperature, grinding the product, and sieving the product with a 200;
s2, taking the matrix particles, washing the matrix particles with deionized water, drying the matrix particles at 105 ℃ for 22 hours, and collecting the dried matrix particles; respectively weighing 47 parts by weight of deionized water, 1 part by weight of 1% hydrochloric acid, 47 parts by weight of epichlorohydrin and 12 parts by weight of dry matrix particles, placing the materials into a beaker, stirring and mixing the materials, adjusting the pH value to 7.0 by using 10% sodium hydroxide, stirring and mixing the materials, collecting a mixed solution, adding sodium carboxymethylcellulose into the mixed solution according to the mass ratio of 1:15, performing ultrasonic dispersion at 250W for 12min, performing heat preservation reaction at 47 ℃ for 7h, filtering and collecting lower-layer precipitates, and drying the lower-layer precipitates for 6-8 h to prepare modified matrix particles;
s3, respectively weighing 47 parts of deionized water, 4 parts of hexadecyl trimethyl ammonium bromide, 7 parts of 5% silver nitrate solution by mass and 7 parts of hydrazine hydrate by weight, stirring and mixing, collecting mixed reaction liquid, dropwise adding the 2% silver nitrate solution by mass into the mixed reaction liquid according to the mass ratio of 1:15, controlling the dropwise adding speed to be 2mL/min, and stirring, mixing and collecting to obtain base body liquid after the dropwise adding is finished; respectively weighing 47 parts by weight of base fluid, 12 parts by weight of TEOS, 4 parts by weight of 10% ammonia water and 27 parts by weight of absolute ethyl alcohol, placing the mixture in a beaker, stirring, mixing, standing for 7 hours, and collecting to obtain a mixed sol solution;
s4, adding the dry matrix particles into the mixed sol solution according to the mass ratio of 1:10, standing for 4 hours, performing ultrasonic dispersion and filtration, collecting a filter cake, drying at 105 ℃ to constant weight, and collecting dry particles to obtain the high-dispersion anti-discoloration nano-silver antibacterial agent material.
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| CN111357767B (en) | 2021-02-23 |
| CN112438274A (en) | 2021-03-05 |
| CN112438274B (en) | 2022-09-02 |
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