CN115948069A - Dual-antibacterial super-lyophobic coating and preparation method thereof - Google Patents
Dual-antibacterial super-lyophobic coating and preparation method thereof Download PDFInfo
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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
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- Paints Or Removers (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the field of antibacterial material preparation, and particularly discloses a dual-antibacterial super-lyophobic coating and a preparation method thereof. According to the invention, the fluorine-containing semi-cage oligomeric silsesquioxane, ethanol, inorganic nanoparticles and antibacterial peptide are doped into the water-based resin, and the prepared double antibacterial super-lyophobic coating has the biological antibacterial effect of the physical antibacterial synergistic antibacterial peptide of the super-lyophobic layer, particularly has a strong repellent effect on water or organic solvents such as glycerol and ethylene glycol, has excellent lyophobic property and antibacterial property, can realize high-efficiency broad-spectrum antibacterial, and has the antibacterial rate of over 99% on escherichia coli and staphylococcus aureus.
Description
Technical Field
The invention belongs to the field of antibacterial material preparation, and particularly relates to a dual-antibacterial super-lyophobic coating and a preparation method thereof.
Background
Currently, the world is suffering from severe challenge of new coronavirus infection, global public health safety is seriously threatened, people pay more attention to health and health, and higher requirements are put on the safety of food packaging and medical appliances. The bacteria, as a kind of microorganism existing in nature, are easy to breed and propagate on the surface of an object, and pose a serious threat to the life and health of human beings. Therefore, it is of great significance to develop a surface material that effectively inhibits the growth of bacteria and is effective in sterilization and virus resistance.
As a special new material, the antibacterial super-lyophobic coating material has special performances of antibiosis, self-cleaning, anti-icing, anticorrosion, antifouling, antiscaling, fluid drag reduction and the like, and has potential application value in many aspects of medical appliances, electronic equipment, traffic facilities, clothing textile and the like, so the antibacterial super-lyophobic coating material is concerned by researchers. In recent years, researchers at home and abroad mainly prepare the antibacterial super-lyophobic coating material by two modes of doping an inorganic antibacterial agent and doping an organic antibacterial agent. For example, patent document 202111573456.3 discloses a durable antibacterial antiviral super-amphiphobic coating and a preparation method thereof, the method comprises the steps of mixing and stirring silicon dioxide nanoparticles, an alcohol solvent, a basic catalyst, silicate ester and a fluorine-containing organic substance according to a corresponding proportion to prepare super-amphiphobic modified nano silicon dioxide particles, then mixing and stirring fluorocarbon resin, acrylic resin, barium sulfate powder, an organic solvent and various auxiliaries to prepare a primer, then stirring and mixing the super-amphiphobic modified nano silicon dioxide particles, superfine nano silver powder and absolute ethyl alcohol to prepare a finish paint, finally spraying the primer paint on a base material, and spraying the finish paint on the primer after the surface of the primer is dried to prepare the durable antibacterial antiviral super-amphiphobic coating, wherein the static contact angles of water and pump oil of the coating are both over 150 degrees, and the antibacterial rates of escherichia coli and staphylococcus aureus are both over 99.9%. Also, for example, patent document No. 201811054100.7 discloses a superhydrophobic antibacterial cationic fluoropolymer nano-coating, in the preparation process of the coating, 3-chloropropene, which is a quaternary amination reagent, and alkyl-dimethyl tertiary amine are subjected to a temperature rise reaction to prepare a propylene-alkyl-dimethyl quaternary ammonium salt monomer, namely an antibacterial cationic monomer, then the antibacterial cationic monomer, a fluorine-containing monomer, a styrene monomer and an acrylic acid monomer are mixed, an antibacterial cationic fluoropolymer microsphere emulsion is prepared through an emulsion polymerization reaction, and finally the superhydrophobic antibacterial cationic fluoropolymer microsphere emulsion is prepared by matching with an aqueous curing agent to obtain the superhydrophobic antibacterial cationic fluoropolymer nano-coating.
Although the antibacterial super-lyophobic coating material prepared by the inorganic antibacterial agent doping mode and the organic antibacterial agent doping mode has good lyophobic property and excellent antibacterial property, realizes double antibacterial effects of physical antibacterial and chemical antibacterial to a certain degree, and has wide application value, however, the two technologies have more defects, for example, the antibacterial super-lyophobic prepared by the inorganic antibacterial agent doping method takes an inorganic silver system as a main antibacterial agent, the production process is complex, the manufacturing is difficult, the cost is high, in addition, the silver system antibacterial agent is easy to change color, and free silver ions on the surface of a product coated with the silver system antibacterial agent super-lyophobic coating are easily reduced into simple substance silver to present gray or brown under the sunlight irradiation condition, so the transmittance of the product is seriously influenced. The super-lyophobic coating prepared by using the organic antibacterial agent doping method has the advantages that the antibacterial agent mainly comprises quaternary ammonium salts, organic metals and the like, the organic antibacterial agent in the antibacterial super-lyophobic coating is easy to decompose and separate out in a solvent environment, decomposition products are toxic, drug resistance and cross resistance are easy to generate, and in addition, the safety of the super-lyophobic coating cannot be determined so far. Therefore, the existing antibacterial super-lyophobic coating technology cannot meet the requirements of industries such as food packaging, medical appliances and the like on safety and stability.
Disclosure of Invention
Aiming at the problem that the antibacterial super-lyophobic coating material in the prior art is poor in safety and stability when applied to industries such as food packaging, medical appliances and the like, the invention provides a double antibacterial super-lyophobic coating and a preparation method thereof.
In order to achieve the purpose, the method specifically comprises the following technical scheme:
a double-antibacterial super-lyophobic coating is prepared from raw materials including fluorine-containing semi-cage type oligomeric silsesquioxane, ethanol, inorganic nanoparticles, antibacterial peptide and water-based resin.
The double-antibacterial super-lyophobic coating has the advantages of physical antibacterial property of the super-lyophobic layer and biological antibacterial property of the antibacterial peptide, can realize high-efficiency broad-spectrum antibacterial property, and has antibacterial rate of over 99% on escherichia coli and staphylococcus aureus.
In a preferred embodiment of the invention, the mass ratio of the fluorine-containing semi-cage type oligomeric silsesquioxane to the ethanol is (15-70) to (30-85).
In a preferred embodiment of the present invention, the mass ratio of the fluorine-containing semi-cage type oligomeric silsesquioxane to the aqueous resin is 1 (20000 to 200000).
As a preferred embodiment of the invention, the mass ratio of the inorganic nanoparticles to the aqueous resin is 1 (50-300).
In a preferred embodiment of the present invention, the mass ratio of the antimicrobial peptide to the aqueous resin is 1 (1000-5000).
As a preferred embodiment of the present invention, the inorganic nanoparticles are at least one of silica nanoparticles, titania nanoparticles, alumina nanoparticles, and zirconia nanoparticles.
As a preferred embodiment of the present invention, the size of the inorganic nanoparticles is 5 to 500nm.
In a preferred embodiment of the present invention, the antimicrobial peptide is at least one of nisin, pediocin, enteromycin and cecropin.
In a preferred embodiment of the invention, the aqueous resin is at least one of aqueous inorganic silicone resin SJ-8050, aqueous silicone resin S-227, aqueous polyacrylate 3958, aqueous polyurethane 2944, aqueous epoxy resin S-969 and aqueous fluorocarbon resin DF-01L.
In the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 0.1-20%.
A preparation method of a dual-antibacterial super-lyophobic coating comprises the following steps:
(1) Mixing and dissolving fluorine-containing semi-cage oligomeric silsesquioxane and ethanol, and performing ultrasonic treatment to obtain a fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution;
(2) Mixing the fluorine-containing semi-cage type oligomeric silsesquioxane ethanol type solution, inorganic nanoparticles, antibacterial peptide and water-based resin to obtain dual-antibacterial super-lyophobic coating slurry;
(3) And coating the dual-antibacterial super-lyophobic coating slurry on a carrier, and curing to obtain the dual-antibacterial super-lyophobic coating.
As a preferred embodiment of the present invention, the ultrasonic frequency of the ultrasonic treatment is 20 to 60kHz.
As a preferred embodiment of the present invention, the time of the ultrasonic treatment is 5 to 60min.
As a preferred embodiment of the present invention, the curing time is 12 to 48 hours.
In a preferred embodiment of the present invention, the carrier is a glass carrier.
In a preferred embodiment of the present invention, the coating is at least one of spray coating, spin coating, brush coating, and roll coating.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention introduces low surface energy substance fluorine-containing semi-cage type oligomeric silsesquioxane and inorganic nano-particles into aqueous resin, and can obtain the ultra-lyophobic coating with physical antibiosis (physically isolating bacteria-containing liquid). The coating has strong repellent effect on water or organic solvents such as glycerin, glycol and the like, and has excellent lyophobicity.
(2) The invention introduces antibacterial peptide into the super lyophobic coating to prepare the synergistic antibacterial super lyophobic coating with physical antibacterial (super lyophobic surface) and biological antibacterial (antibacterial peptide). Wherein, the coating can realize high-efficiency broad-spectrum antibiosis only by doping a proper amount of antibacterial peptide, and the antibacterial rate to escherichia coli and staphylococcus aureus is over 99 percent.
(3) The preparation process of the dual-antibacterial super-lyophobic coating uses environment-friendly and non-toxic solvents such as water, ethanol and the like, relates to the simple and easy-to-operate equipment, can be realized by simple construction such as spraying, brushing, roller coating and the like, has high construction efficiency and low preparation cost, and is expected to be applied to the industry fields of food packaging, medical appliances and the like.
Drawings
Fig. 1 is an appearance view of a dual antimicrobial ultralyophobic coating slurry in example 1 of the present invention.
Fig. 2 is a view of the surface of a dual antibacterial ultralyophobic coating in example 1 of the present invention dropped with 10 μ L of water drop (left) and 10 μ L of ethylene glycol drop (right), respectively.
FIG. 3 is a graph showing the antibacterial effect of the blank control group in the antibacterial test in example 1 of the present invention.
Fig. 4 is a graph showing the antibacterial effect of the dual antibacterial ultralyophobic coating in example 1 of the present invention.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described by the following specific examples.
In the implementation of the invention and the comparative example, the absolute ethyl alcohol and the inorganic nano particles are all commercially available analytical pure reagents.
The fluorine-containing semi-cage type oligomeric silsesquioxane can be obtained by self-manufacture or market purchase, the fluorine-containing semi-cage type oligomeric silsesquioxane used in the following examples and comparative examples is of the same type, and the preparation process can be found in patent document CN202010348435.0:
step 1: uniformly mixing 1H,2H and 2H-perfluoro alkoxy silane, sodium hydroxide and absolute ethyl alcohol, dropwise adding deionized water, heating and stirring for reaction, rotationally evaporating an ethanol solvent after the reaction is finished, and performing vacuum drying to obtain fluorine-containing semi-cage type oligomeric silsesquioxane sodium salt;
step 2: adding the fluorine-containing semi-cage type oligomeric silsesquioxane sodium salt into concentrated hydrochloric acid in batches, reacting at room temperature, filtering to remove insoluble substances after the reaction is finished, dripping the filtrate into crushed ice to separate out white solid, and then washing with water and alcohol, and drying in vacuum to obtain the fluorine-containing semi-cage type oligomeric silsesquioxane.
In the examples of the present invention and the comparative examples, the size of the inorganic nanoparticles was 5 to 500nm.
In the examples and the comparative examples of the invention, the ultrasonic frequency of the fluorine-containing semi-cage type oligomeric silsesquioxane ethanol type solution is 20-60kHz.
In the examples and comparative examples of the present invention, the room temperature standing time for which the slurry was uniformly coated on the glass sheet was 12 to 48 hours.
In the examples of the present invention and the comparative examples, the solid content of the aqueous resin in the coating layer was 0.1 to 20%.
Example 1
The preparation raw materials of the double-antibacterial super-lyophobic coating comprise fluorine-containing semi-cage oligomeric silsesquioxane, absolute ethyl alcohol, inorganic nanoparticles, antibacterial peptide and water-based resin;
the inorganic nanoparticles are silica nanoparticles; the size of the inorganic nano-particles is 5-500nm;
the antibacterial peptide is nisin (CAS: 1414-45-5, molecular weight 3354.07);
the water-based resin is water-based inorganic silicon resin SJ-8050;
in the double-antibacterial super-lyophobic coating, the mass content (solid content) of the water-based inorganic silicone resin is 0.1%.
The preparation method of the dual-antibacterial super-lyophobic coating comprises the following steps:
(1) Mixing and stirring fluorine-containing semi-cage type oligomeric silsesquioxane and absolute ethyl alcohol for dissolving, and then treating for 30min under 20kHz ultrasonic wave to prepare a fluorine-containing semi-cage type oligomeric silsesquioxane ethanol solution, wherein the mass content of the fluorine-containing semi-cage type oligomeric silsesquioxane is 15%;
(2) Adding a fluorine-containing semi-cage oligomeric silsesquioxane ethanol-type solution, inorganic nanoparticles and antibacterial peptide into aqueous resin, and uniformly mixing to obtain a dual-antibacterial super-lyophobic coating slurry, wherein the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol-type solution to the aqueous resin is 1; the appearance is shown in figure 1;
(3) Uniformly spraying and coating the slurry of the double-antibacterial super-lyophobic coating on a glass sheet, standing at room temperature for 24 hours, and naturally airing and curing to obtain the double-antibacterial super-lyophobic coating; the appearance is shown in fig. 2.
Example 2
Compared with example 1, the differences are:
the inorganic nanoparticles are titanium dioxide nanoparticles;
the antibacterial peptide is pediocin;
the water-based resin is water-based organic silicon resin S-227;
in the double antibacterial super-lyophobic coating, the solid content of the water-based resin is 2 percent.
The mass content of the fluorine-containing semi-cage oligomeric silsesquioxane in the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution is 20%.
The mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution to the aqueous resin is 1;
the mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol type solution is 30kHz;
the slurry is uniformly coated on the glass sheet and is placed for 12 hours at room temperature;
the coating method is spin coating.
Example 3
Compared with example 1, the differences are:
the inorganic nano-particles are aluminum oxide nano-particles;
the antibacterial peptide is enteromycin;
the water-based resin is water-based fluorocarbon resin DF-01L;
in the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 5 percent;
the mass content of the fluorine-containing semi-cage oligomeric silsesquioxane in the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution is 25 percent;
the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution to the aqueous resin is 1;
the mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol type solution is 40kHz;
the slurry is uniformly coated on the glass sheet and is placed for 36 hours at room temperature;
the coating mode is brush coating.
Example 4
Compared with example 1, the difference is that:
the inorganic nano-particles are zirconium dioxide nano-particles;
the antibacterial peptide is cecropin;
the water-based resin is water-based polyacrylate 3958;
in the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 10 percent;
the mass content of the fluorine-containing semi-cage oligomeric silsesquioxane in the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution is 30 percent;
the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution to the aqueous resin is 1;
the mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol type solution is 50kHz;
the slurry is uniformly coated on the glass sheet and is placed for 48 hours at room temperature;
the coating mode is roller coating.
Example 5
Compared with example 1, the differences are:
the inorganic nanoparticles are silica nanoparticles;
the antibacterial peptide is pediocin;
the waterborne resin is waterborne polyurethane 2944;
in the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 12%;
the mass content of the fluorine-containing semi-cage oligomeric silsesquioxane in the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution is 35 percent;
the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution to the aqueous resin is 1;
the mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol type solution is 60kHz;
the room-temperature standing time of the slurry uniformly coated on the glass sheet is 16h;
the coating mode is spraying.
Example 6
Compared with example 1, the difference is that:
the inorganic nanoparticles are titanium dioxide nanoparticles;
the antibacterial peptide is enteromycin;
the water-based resin is water-based epoxy resin S-969;
in the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 14 percent;
the mass content of the fluorine-containing semi-cage oligomeric silsesquioxane in the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution is 40%.
The mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol-type solution to the aqueous resin is 1.
The mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol type solution is 30kHz;
the slurry is uniformly coated on the glass sheet and is placed for 20 hours at room temperature;
the coating method is spin coating.
Example 7
Compared with example 1, the difference is that:
the inorganic nano-particles are aluminum oxide nano-particles;
the antibacterial peptide is cecropin;
the water-based resin is water-based inorganic silicon resin SJ-8050;
in the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 15 percent;
the fluorine-containing semi-cage type oligomeric silsesquioxane in the fluorine-containing semi-cage type oligomeric silsesquioxane ethanol type solution accounts for 45% by mass;
the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution to the aqueous resin is 1;
the mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol type solution is 40kHz;
the room temperature standing time of the slurry evenly coated on the glass sheet is 22h;
the coating mode is brush coating.
Example 8
Compared with example 1, the difference is that:
the inorganic nano-particles are zirconium dioxide nano-particles; the size of the inorganic nano-particles is 5-500nm;
the antibacterial peptide is nisin;
the water-based resin is water-based organic silicon resin S-227;
in the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 16 percent;
the mass content of the fluorine-containing semi-cage oligomeric silsesquioxane in the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution is 50 percent;
the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution to the aqueous resin is 1;
the mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol type solution is 50kHz;
the room temperature standing time of the slurry evenly coated on the glass sheet is 28h;
the coating mode is roller coating.
Example 9
Compared with example 1, the differences are:
the inorganic nanoparticles are silica nanoparticles;
the antibacterial peptide is pediocin;
the water-based resin is water-based fluorocarbon resin DF-01L;
in the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 16.5 percent;
the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution to the aqueous resin is 1;
the mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution is 60kHz;
the slurry is uniformly coated on the glass sheet and is placed for 30 hours at room temperature;
the coating mode is spraying.
Example 10
Compared with example 1, the differences are:
the inorganic nanoparticles are titanium dioxide nanoparticles;
the antibacterial peptide is enteromycin;
the water-based resin is water-based polyacrylate 3958;
in the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 17 percent;
the mass content of the fluorine-containing semi-cage oligomeric silsesquioxane in the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution is 60 percent;
the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution to the aqueous resin is 1;
the mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol type solution is 20kHz;
the room temperature standing time of the slurry evenly coated on the glass sheet is 32h;
the coating method is spin coating.
Example 11
Compared with example 1, the difference is that:
the inorganic nano-particles are aluminum oxide nano-particles;
the antibacterial peptide is cecropin;
the waterborne resin is waterborne polyurethane 2944;
in the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 18 percent;
the mass content of the fluorine-containing semi-cage oligomeric silsesquioxane in the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution is 65%;
the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution to the aqueous resin is 1;
the mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol type solution is 30kHz;
the room-temperature standing time of the slurry uniformly coated on the glass sheet is 35h;
the coating mode is brush coating.
Example 12
Compared with example 1, the difference is that:
the inorganic nano-particles are zirconium dioxide nano-particles;
the antibacterial peptide is nisin;
the water-based resin is water-based epoxy resin S-969;
in the double-antibacterial super-lyophobic coating, the solid content of the water-based resin is 20 percent;
the mass content of the fluorine-containing semi-cage oligomeric silsesquioxane in the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution is 70%;
the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution to the aqueous resin is 1;
the mass ratio of the inorganic nanoparticles to the aqueous resin is 1;
the mass ratio of the antibacterial peptide to the aqueous resin is 1;
the ultrasonic frequency of the fluorine-containing semi-cage oligomeric silsesquioxane ethanol type solution is 40kHz;
the room temperature standing time of the slurry evenly coated on the glass sheet is 38h;
the coating mode is roller coating.
Comparative example 1
Compared with example 1, the difference is that: this comparative example did not add the fluorine-containing semi-cage oligomeric silsesquioxane.
Comparative example 2
Compared with example 1, the difference is that: no antimicrobial peptide was added to this comparative example.
Comparative example 3
Compared with example 1, the difference is that: this comparative example did not add antimicrobial peptide and fluoro-containing semi-cage oligomeric silsesquioxane.
And (3) detecting the antibacterial activity of the double antibacterial super lyophobic coating:
coating sample preparation for examples and comparative examples: for each sample, 3 PET films were prepared for coating with the dual antimicrobial ultralyophobic coating, and 1 PET film of the slurry without antimicrobial treatment was prepared as a control. (Note: use of 3 or more samples subjected to antibacterial treatment contributes to reduction of errors) A base PET film and a cover PET film having a size of (50. + -.2) mm X (50. + -.2) mm and a size of (40. + -.2) mm X (40. + -.2) mm were prepared, respectively. During sample preparation, care is taken to avoid contamination of the sample by microorganisms or organic matter. The test specimens were cleaned, disinfected or sterilized (70% alcohol scrub) prior to testing.
The Staphylococcus aureus stock (200. Mu.L) was added to a test tube containing sterile Luria-Bertani (LB) broth (10 mL), and then cultured in an incubator at 170rpm at 30 ℃ for 20-24 hours, and the LB broth was used to dilute the stock to a concentration of 6.0X 10 5 CFU/mL. For each sample (control and experimental groups in sample preparation), a staphylococcus aureus culture (400. Mu.L) was inoculated onto a (50. + -.2) mmX (50. + -.2) mm bottom PET film and a (40. + -.2) mmX (40. + -.2) mm cover film was placed over the inoculum, and the inoculum was spread by pressing the film slightly downward to ensure that the inoculum did not overflow from the edges of the film. After incubation at 37 ℃ for 24h, 0.1ml of the broth was aspirated from the membrane and then serially diluted ten-fold with LB broth. Finally, 100. Mu.L of the diluted solution was spread on agar medium and incubated at 37 ℃ for 24 hours, and bacterial colonies were counted for each sample. Three groups of antibacterial experiments were performed simultaneously for each sample, and the average value was used as the experimental result. The calculation of the bacterial inhibition rate is disclosed as follows:
wherein R is the bacteriostasis rate, and M and N are the colony numbers on the culture mediums of a blank control group and an experimental investigation group respectively.
In the case of surface colonies in the blank control group of example 1, as shown in FIG. 3, a large number of colonies appeared on the surface of the medium. The bacteriostatic effect of the double-antibacterial ultralyophobic coating in example 1 is shown in fig. 4, the number of colonies on the surface of the culture medium is 6, and the bacteriostatic rate reaches 99.6%.
The bacteriostatic effects of the coating samples of examples and comparative examples are shown in table 1.
TABLE 1 bacteriostatic effect of coating samples of examples and comparative examples
According to the bacteriostatic effect of the coating, the bacteriostatic effect of the double-antibacterial super-lyophobic coating on staphylococcus aureus is more than 99%.
Contact and rolling angle testing:
the coatings prepared in examples and comparative examples were left at room temperature and tested for contact angles of water (10. Mu.L) and ethylene glycol (10. Mu.L) after 48 hours, and the results are shown in Table 2.
Table 1 coating contact angle, sliding angle results for examples and comparative examples
| Water contact angle | Water rolling angle | Ethylene glycol contact angle | Rolling angle of ethylene glycol | |
| Example 1 | 162.7° | 1.7° | 153.2° | 14.8° |
| Example 2 | 160.4° | 1.2° | 152.5° | 15.2° |
| Example 3 | 163.5° | 1.9° | 156.1° | 13.4° |
| Example 4 | 157.3° | 2.6° | 153.8° | 19.3° |
| Example 5 | 160.7° | 3.7° | 156.3° | 16.7° |
| Example 6 | 164.3° | 4.2° | 152.8° | 13.4° |
| Example 7 | 158.4° | 5.1° | 155.7° | 14.6° |
| Example 8 | 161.3° | 3.2° | 156.1° | 13.9° |
| Example 9 | 162.5° | 2.3° | 154.2° | 12.8° |
| Example 10 | 161.8° | 2.7° | 155.7° | 16.5° |
| Example 11 | 159.6° | 3.4° | 153.1° | 12.7° |
| Example 12 | 162.9° | 1.9° | 152.9° | 17.3° |
| Comparative example 1 | 124.3° | 22.3° | 103.4° | 35.2° |
| Comparative example 2 | 154.9° | 5.1° | 151.8 | 15.5° |
| Comparative example 3 | 122.5° | 21.9° | 106.1° | 32.4° |
From the contact angle and rolling angle results of the examples, it can be seen that the dual antimicrobial ultralyophobic coating of the present invention has a strong repellent effect on water and ethylene glycol.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The double-antibacterial super-lyophobic coating is characterized in that the preparation raw materials comprise fluorine-containing semi-cage oligomeric silsesquioxane, ethanol, inorganic nanoparticles, antibacterial peptide and water-based resin.
2. The dual antimicrobial ultralyophobic coating of claim 1, wherein the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane to the aqueous resin is 1 (20000-200000).
3. The dual antimicrobial ultralyophobic coating of claim 1, wherein the mass ratio of the antimicrobial peptide to the aqueous resin is 1 (1000-5000).
4. The dual antimicrobial ultralyophobic coating of claim 1, wherein the mass ratio of the inorganic nanoparticles to the aqueous resin is 1 (50-300).
5. The dual antimicrobial ultralyophobic coating of claim 1, wherein the mass ratio of the fluorine-containing semi-cage oligomeric silsesquioxane to ethanol is (15-70) to (30-85).
6. The dual antimicrobial ultralyophobic coating of claim 1, wherein the inorganic nanoparticles are at least one of silica nanoparticles, titania nanoparticles, alumina nanoparticles, and zirconia nanoparticles; the size of the inorganic nano-particles is 5-500nm.
7. The dual antimicrobial ultralyophobic coating of claim 1, wherein the antimicrobial peptide is at least one of nisin, pediocin, enteromycin, cecropin.
8. The dual antimicrobial ultralyophobic coating of claim 1, wherein the aqueous resin is at least one of aqueous inorganic silicone resin SJ-8050, aqueous silicone resin S-227, aqueous polyacrylate 3958, aqueous polyurethane 2944, aqueous epoxy resin S-969, aqueous fluorocarbon resin DF-01L.
9. The method of preparing a dual antimicrobial ultralyophobic coating according to any one of claims 1 to 8, comprising the steps of:
(1) Mixing and dissolving fluorine-containing semi-cage oligomeric silsesquioxane and ethanol, and performing ultrasonic treatment to obtain a fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution;
(2) Mixing the fluorine-containing semi-cage oligomeric silsesquioxane ethanol solution, inorganic nanoparticles, antibacterial peptide and aqueous resin to obtain dual-antibacterial super-lyophobic coating slurry;
(3) And coating the dual-antibacterial super-lyophobic coating slurry on a carrier, and curing to obtain the dual-antibacterial super-lyophobic coating.
10. The method of preparing a dual antimicrobial ultralyophobic coating of claim 9, wherein the ultrasonic frequency of the ultrasonic treatment is 20-60kHz; the ultrasonic treatment time is 5-60min; the curing time is 12-48h; the coating mode is at least one of spraying, spin coating, brush coating and roller coating.
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| CN106433364A (en) * | 2016-09-22 | 2017-02-22 | 南开大学 | Superhydrophobicity coating based on waterborne emulsion and preparing method and application thereof |
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| CN106433364A (en) * | 2016-09-22 | 2017-02-22 | 南开大学 | Superhydrophobicity coating based on waterborne emulsion and preparing method and application thereof |
| CN106585034A (en) * | 2016-11-29 | 2017-04-26 | 昆山洁宏无纺布制品有限公司 | Antibacterial and antifouling medical table cloth and manufacturing method of same |
| CN111499869A (en) * | 2020-04-27 | 2020-08-07 | 株洲绿智新材料科技有限公司 | Fluorinated semi-cage silsesquioxane and preparation method and application thereof |
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