CN114868768A - Composite antibacterial material, preparation method and application - Google Patents
Composite antibacterial material, preparation method and application Download PDFInfo
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- CN114868768A CN114868768A CN202210443271.9A CN202210443271A CN114868768A CN 114868768 A CN114868768 A CN 114868768A CN 202210443271 A CN202210443271 A CN 202210443271A CN 114868768 A CN114868768 A CN 114868768A
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Abstract
The invention relates to the technical field of antibacterial materials, in particular to a composite antibacterial material and a preparation method and application thereof. The composite antibacterial material provided by the invention comprises the silver nanowires and the zinc oxide shell layers coated on the surfaces of the silver nanowires, and has excellent antibacterial and antiviral properties.
Description
Technical Field
The invention relates to the technical field of antibacterial materials, in particular to a composite antibacterial material and a preparation method and application thereof.
Background
The antibacterial material includes natural antibacterial material, organic antibacterial material and inorganic antibacterial material. The inorganic antibacterial material is a novel antibacterial material, has the advantages of wide antibacterial spectrum, lasting antibacterial effect, excellent high-temperature resistance and the like compared with natural antibacterial materials and organic antibacterial materials, and does not cause drug resistance of thalli in the using process.
Silver is an inorganic antibacterial material with broad-spectrum antibacterial property, and silver ions can destroy cell membrane at a certain concentrationOr reducing the activity of bioactive enzyme, and has good inhibitory effect on gram-positive bacteria, gram-negative bacteria, fungi, etc. Zinc oxide is another inorganic antibacterial material that is capable of producing active oxygen (primarily H) by catalyzing substances such as water or oxygen in the environment 2 O 2 ) The active oxygen can chemically react with the membrane protein, thereby exerting an antibacterial effect.
In the related art, silver nitrate is usually added into a zinc salt solution to be doped to prepare an Ag/ZnO composite material in which silver nanoparticles are mixed with zinc oxide nanoparticles, so as to be used as an antibacterial material. However, in the course of carrying out the present invention, the inventors found that the above Ag/ZnO composite material still has poor antibacterial properties.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect of poor antibacterial performance of the Ag/ZnO composite material in the prior art, thereby providing the composite antibacterial material, the preparation method and the application.
The inventor of the present invention has found that the main reason why the Ag/ZnO composite material in the related art has poor antibacterial performance is that the Ag/ZnO composite material is formed by mixing silver nanoparticles and zinc oxide nanoparticles, most of the silver nanoparticles or zinc oxide nanoparticles exist in the form of an aggregate, and only a small portion of the silver nanoparticles and the zinc oxide nanoparticles contact each other to form a heterostructure, so that the antibacterial performance of the Ag/ZnO composite material is mainly the simple superposition of the antibacterial performance of the silver nanoparticles and the antibacterial performance of the zinc oxide nanoparticles.
Therefore, the invention provides a composite antibacterial material which comprises a silver nanowire and a zinc oxide shell layer coated on the surface of the silver nanowire.
Optionally, the diameter of the silver nanowire is 30-100 nm, and the length of the silver nanowire is 1-100 μm; the thickness of the zinc oxide shell layer is 10-700 nm.
The invention also provides a method for preparing the composite antibacterial material, which comprises the following operations:
mixing silver nanowire, zinc salt and triethanolamine in a solution, and carrying out hydrothermal reaction under an ultrasonic condition.
Optionally, the power of the ultrasound is 200-400W, and the frequency is 10 MHz-80 MHz.
Optionally, the temperature of the hydrothermal reaction is 40-90 ℃, and the time is 0.5-6 h.
Optionally, the mixing silver nanowires, zinc salt, and triethanolamine in a solution includes:
adding silver nanowires into a solution containing zinc salt and triethanolamine;
optionally, the solution is an aqueous solution.
Optionally, after the silver nanowire, the zinc salt and the triethanolamine are mixed in the solution, the molar ratio of the zinc ions to the triethanolamine is 1 (100-1000), and the molar ratio of the silver to the zinc ions is 1: (2-32);
optionally, the zinc salt is selected from zinc acetate and/or zinc nitrate.
Optionally, the method further comprises an operation of washing the silver nanowires with an organic solvent;
optionally, the cleaning is ultrasonic cleaning, the power of the ultrasonic is 200-400W, and the frequency is 10-80 MHz;
optionally, the organic solvent is at least one selected from the group consisting of absolute ethanol, acetone, methanol, ethyl acetate, and toluene.
The invention also provides the composite antibacterial material or the application of the composite antibacterial material prepared by the method in preparing antibacterial products and/or antiviral products.
Optionally, the use is in the preparation of an antibacterial coating, a water treatment product or a biological antibacterial material; optionally, the antimicrobial product comprises an anti-escherichia coli product and/or an anti-staphylococcus aureus product.
The technical scheme of the invention has the following advantages:
1. the composite antibacterial material provided by the invention comprises the silver nanowires and the zinc oxide shell layers coated on the surfaces of the silver nanowires, and has excellent antibacterial and antiviral properties. Specifically, in the composite antibacterial material, the zinc oxide shell layer is uniformly coated on the surface of the silver nanowire, silver is mainly used as a reinforcing agent of the photocatalytic performance of the zinc oxide and forms a heterostructure with the zinc oxide, a plasma resonance effect exists between the silver and the zinc oxide in the heterostructure, and the separation of electron-hole pairs can be promoted, so that the photocatalytic efficiency of the zinc oxide is improved, the photocatalytic antibacterial and antiviral performance of the zinc oxide is obviously improved, and meanwhile, the silver nanowire coated in the zinc oxide shell layer can also play part of the antiviral performance. Therefore, compared with the simple mixing of the silver nanoparticles and the zinc oxide nanoparticles, the composite antibacterial material has excellent antibacterial and antiviral properties.
2. According to the composite antibacterial material provided by the invention, the zinc oxide shell layer is coated on the surface of the silver nanowire, so that on one hand, the zinc oxide shell layer can effectively inhibit silver ions in the silver nanowire from excessively overflowing to avoid the situation that the excessive silver ions threaten the health and safety of organisms, and on the other hand, the zinc oxide shell layer has good biocompatibility and biological safety, so that the composite antibacterial material has good biocompatibility and biological safety.
3. According to the method for preparing the composite antibacterial material, provided by the invention, by carrying out hydrothermal reaction under an ultrasonic condition, on one hand, agglomeration of zinc oxide generated by the reaction can be effectively avoided, and on the other hand, the zinc oxide generated by the reaction can be uniformly coated on the surface of the silver nanowire, so that the method can effectively avoid simple mixing of the zinc oxide and the silver nanowire, and thus the Ag/ZnO heterostructure with excellent performance is prepared.
4. According to the method for preparing the composite antibacterial material, the silver nanowires are cleaned by using the organic solvent, so that pollutants on the surfaces of the silver nanowires can be removed, the silver nanowires with clean surfaces can be obtained, the binding force between the silver nanowires and zinc oxide is obviously enhanced, and a stable core-shell structure is formed.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a SEM test result chart of the composite antibacterial material prepared in example 1 of the present invention;
FIG. 2 is a TEM image of the composite antibacterial material prepared in example 1 of the present invention;
fig. 3 is a SEM examination result diagram of the composite antibacterial material prepared in comparative example 1 of the present invention.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
The raw materials and reagents involved in the embodiment of the invention are as follows:
zinc acetate (manufacturer: alatin, lot number: Z110777);
triethanolamine (manufacturer: Allantin, lot number: T108151);
silver nanowires (manufacturer: Aladdin, batch: S301965).
Example 1
The embodiment provides a method for preparing a composite antibacterial material, which comprises the following operations:
(1) dissolving 0.23mmol of zinc acetate dihydrate in 50ml of water, adding 150mmol of triethanolamine, and stirring until the solution is transparent to obtain an aqueous solution of zinc acetate and triethanolamine;
(2) putting silver nanowires (diameter 70nm and length 20 μm) in an organic solvent (absolute ethyl alcohol) and ultrasonically cleaning (200W, 20MHz) for 0.5 h;
(3) and (3) adding 0.0093mmol of the silver nanowire cleaned in the operation (2) into the aqueous solution of zinc acetate and triethanolamine obtained in the operation (1), heating under the ultrasonic (200W, 20MHz) condition, and carrying out hydrothermal reaction at the reaction temperature of 60 ℃ for 2h to obtain the ZnO coated silver nanowire composite antibacterial material.
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, wherein the scanning electron microscope detection result is shown in fig. 1, and the transmission electron microscope detection result is shown in fig. 2. As can be seen from fig. 1 and 2, the composite antibacterial material prepared in this embodiment is composed of a silver nanowire and a zinc oxide shell layer coated on the surface of the silver nanowire, and the silver nanowire and the zinc oxide shell layer form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 200-400 nm.
Example 2
A composite antibacterial material was prepared using the method of example 1, except that: in operation (3) of this example, the power of the ultrasound was 200W and the frequency was 10 MHz.
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, and the detection results show that the composite antibacterial material prepared in the embodiment is composed of silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires, and the silver nanowires and the zinc oxide shell layers form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 200-400 nm.
Example 3
A composite antibacterial material was prepared using the method of example 1, except that: in operation (3) of this example, the power of the ultrasound was 400W and the frequency was 80 MHz.
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, and the detection results show that the composite antibacterial material prepared in the embodiment is composed of silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires, and the silver nanowires and the zinc oxide shell layers form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 200-400 nm.
Example 4
A composite antibacterial material was prepared using the method of example 1, except that: in the operation (3) of this example, the hydrothermal reaction was carried out at a temperature of 40 ℃ for 0.5 hour.
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, and the detection results show that the composite antibacterial material prepared in the embodiment is composed of silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires, and the silver nanowires and the zinc oxide shell layers form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 10-200 nm.
Example 5
A composite antibacterial material was prepared using the method of example 1, except that: in the operation (3) of this example, the hydrothermal reaction was carried out at a temperature of 90 ℃ for 6 hours.
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, and the detection results show that the composite antibacterial material prepared in the embodiment is composed of silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires, and the silver nanowires and the zinc oxide shell layers form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 400-700 nm.
Example 6
A composite antibacterial material was prepared using the method of example 1, except that: in this example, the amounts of the raw materials are: 0.23mmol of zinc acetate dihydrate, 150mmol of triethanolamine and 0.115mmol of silver nanowire.
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, and the detection results show that the composite antibacterial material prepared in the embodiment is composed of silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires, and the silver nanowires and the zinc oxide shell layers form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 200-400 nm.
Example 7
A composite antibacterial material was prepared using the method of example 1, except that: in this example, the amounts of the raw materials are: 0.23mmol of zinc acetate dihydrate, 150mmol of triethanolamine and 0.0072mmol of silver nanowire.
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, and the detection results show that the composite antibacterial material prepared in the embodiment is composed of silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires, and the silver nanowires and the zinc oxide shell layers form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 200-400 nm.
Example 8
A composite antibacterial material was prepared using the method of example 1, except that: in this example zinc acetate was replaced by an equimolar amount of zinc nitrate.
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, and the detection results show that the composite antibacterial material prepared in the embodiment is composed of silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires, and the silver nanowires and the zinc oxide shell layers form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 200-400 nm.
Example 9
A composite antibacterial material was prepared using the method of example 1, except that: in this example, the silver nanowires were not subjected to ultrasonic cleaning in operation (2).
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, and the detection results show that the composite antibacterial material prepared in the embodiment is composed of silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires, and the silver nanowires and the zinc oxide shell layers form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 200-400 nm.
Example 10
A composite antibacterial material was prepared using the method of example 1, except that: in this example, the amounts of the raw materials are: 0.23mmol of zinc acetate dihydrate, 23mmol of triethanolamine and 0.0093mmol of silver nanowire.
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, and the detection results show that the composite antibacterial material prepared in the embodiment is composed of silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires, and the silver nanowires and the zinc oxide shell layers form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 200-400 nm.
Example 11
A composite antibacterial material was prepared using the method of example 1, except that: in this example, the amounts of the raw materials are: 0.23mmol of zinc acetate dihydrate, 230mmol of triethanolamine and 0.0093mmol of silver nanowire.
The composite antibacterial material prepared in the embodiment is subjected to scanning electron microscope detection and transmission electron microscope detection, and the detection results show that the composite antibacterial material prepared in the embodiment is composed of silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires, and the silver nanowires and the zinc oxide shell layers form a core-shell heterostructure. Statistical analysis is carried out on the detection result of the scanning electron microscope and the detection result of the transmission electron microscope, and the thickness of a zinc oxide shell layer in the composite antibacterial material can be determined to be 200-400 nm.
Comparative example 1
A composite antibacterial material was prepared using the method of example 1, except that: in the comparative example (3), no ultrasonic treatment was performed during the hydrothermal reaction.
Scanning electron microscope detection is carried out on the composite antibacterial material prepared in the comparative example, the detection result is shown in fig. 3, and as can be seen from fig. 3, a large number of zinc oxide particles in an aggregated state exist in the composite antibacterial material prepared in the comparative example.
Comparative example 2
The Ag/ZnO composite material is prepared according to the following method:
adding a silver nitrate aqueous solution containing 0.5mol/L of silver nitrate into a zinc acetate aqueous solution containing 0.5mol/L of zinc acetate, wherein the volume ratio of the silver nitrate aqueous solution to the zinc acetate aqueous solution is 1:24.7, reacting for 20min at 80 ℃, cooling the obtained sample to room temperature, performing centrifugal separation, and drying for 30min at 50 ℃ in an oven to obtain the Ag/ZnO composite material.
Comparative example 3
The Ag/ZnO composite material is prepared according to the following method:
adding an aqueous solution containing 0.15mol/L ZnO into a 0.1mol/L silver nitrate aqueous solution, wherein the volume ratio of the silver nitrate aqueous solution to the ZnO aqueous solution is 1:16.47, then irradiating for 10 minutes by using two 9W ultraviolet lamps (lambda is 365nm), centrifuging the obtained sample, and drying for 30min at 50 ℃ in an oven to obtain the Ag/ZnO nanowire composite material.
Examples of the experiments
The experimental example is used for verifying the antibacterial effect of the composite antibacterial material.
The composite antibacterial materials prepared in the examples 1-9 and the comparative examples 1-3 are used for carrying out disinfection experiments on escherichia coli (ATCC8739) and staphylococcus aureus (ATCC 6538P), and the specific method comprises the following steps:
preparing the composite antibacterial material into an aqueous solution with the solution concentration of 1g/L to prepare the antibacterial material with the bacteria concentration of 10 -6 Bacterial suspension per ml. Adding 1mL of bacterial liquid into the test tube, and then adding 1mL of prepared composite antibacterial material aqueous solution. The test tube is fully vibrated, so that the liquid in the test tube is fully contacted. 1mL of the liquid was removed from the tube by a sterilized pipette and placed in a petri dishAnd taking 10mL of the culture medium which is melted and cooled to about 50 ℃ by using a sterilized pipette, putting the culture medium into a culture dish, horizontally placing the culture dish on an experiment table, rotating the culture dish clockwise and anticlockwise to and fro to ensure that the culture medium and the bacterial liquid are fully mixed uniformly, and condensing to obtain a flat plate serving as a treatment group flat plate. And replacing the composite antibacterial material aqueous solution with 1mL of purified water, and repeating the operation to obtain a control group flat plate. The treated plate and the control plate are inversely placed in a biochemical incubator and are cultured for 24 hours at 37 ℃, the number of bacteria is counted respectively, and the sterilization rate is calculated according to the following formula:
the sterilization rate is (number of bacteria in control group-number of bacteria in treatment group)/number of bacteria in control group × 100%.
The results of the experiment are shown in table 1.
TABLE 1 antibacterial Effect of each composite antibacterial Material on Escherichia coli and Staphylococcus aureus
As can be seen from table 1, the composite antibacterial material of the present invention has excellent antibacterial properties, compared to a simple mixture of silver nanoparticles and zinc oxide nanoparticles, and a zinc oxide nanowire coated with silver nanoparticles.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. The composite antibacterial material is characterized by comprising silver nanowires and zinc oxide shell layers coated on the surfaces of the silver nanowires.
2. The composite antibacterial material according to claim 1, wherein the silver nanowires have a diameter of 30 to 100nm and a length of 1 to 100 μm; the thickness of the zinc oxide shell layer is 10-700 nm.
3. A method for preparing the composite antibacterial material of claim 1 or 2, characterized by comprising the following operations:
mixing silver nanowire, zinc salt and triethanolamine in a solution, and carrying out hydrothermal reaction under an ultrasonic condition.
4. The method of claim 3, wherein the power of the ultrasound is 200-400W, and the frequency is 10-80 MHz.
5. The method according to claim 3, wherein the temperature of the hydrothermal reaction is 40-90 ℃ and the time is 0.5-6 h.
6. The method of claim 3, wherein mixing silver nanowires, zinc salt, and triethanolamine in a solution comprises:
adding silver nanowires into a solution containing zinc salt and triethanolamine;
optionally, the solution is an aqueous solution.
7. The method of claim 6, wherein after the silver nanowires, the zinc salt, and the triethanolamine are mixed in the solution, the molar ratio of zinc ions to triethanolamine is 1: (100-1000), wherein the molar ratio of silver to zinc ions is 1: (2-32);
optionally, the zinc salt is selected from zinc acetate and/or zinc nitrate.
8. The method according to claim 3, further comprising an operation of washing the silver nanowires with an organic solvent;
optionally, the cleaning is ultrasonic cleaning, the power of the ultrasonic is 200-400W, and the frequency is 10-80 MHz;
optionally, the organic solvent is at least one selected from the group consisting of absolute ethanol, acetone, methanol, ethyl acetate, and toluene.
9. Use of the composite antibacterial material of claim 1 or 2, or the composite antibacterial material prepared by the method of any one of claims 3 to 8, in the preparation of antibacterial and/or antiviral products.
10. Use according to claim 9, characterized in that it is a use in the preparation of an antibacterial coating, a water treatment product or a bio-antibacterial material;
optionally, the antimicrobial product comprises an anti-escherichia coli product and/or an anti-staphylococcus aureus product.
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