CN115444860A - Nano-silver-loaded antibacterial composite material and preparation method thereof - Google Patents
Nano-silver-loaded antibacterial composite material and preparation method thereof Download PDFInfo
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- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/38—Silver; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/32—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. carbomers, poly(meth)acrylates, or polyvinyl pyrrolidone
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/34—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyesters, polyamino acids, polysiloxanes, polyphosphazines, copolymers of polyalkylene glycol or poloxamers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/42—Proteins; Polypeptides; Degradation products thereof; Derivatives thereof, e.g. albumin, gelatin or zein
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/70—Web, sheet or filament bases ; Films; Fibres of the matrix type containing drug
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/70—Web, sheet or filament bases ; Films; Fibres of the matrix type containing drug
- A61K9/7007—Drug-containing films, membranes or sheets
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
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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 discloses a nano-silver-loaded antibacterial composite material and a preparation method thereof, and relates to the technical field of biological medicines. The preparation method comprises the following steps: the plant extract curcumin or quercetin is compounded into the nano-fiber or membrane material as a reducing agent, then the biomedical material loaded with the plant extract is placed into a silver nitrate aqueous solution with a certain concentration, and the nano-silver-loaded antibacterial composite material is successfully prepared through the in-situ reduction effect of the plant extract on silver nitrate. According to the invention, the plant extract is loaded on carriers such as polymer nano fibers or membranes, so that the method not only can be used for in-situ synthesis of nano silver, but also can be used for preparing a silver-loaded medical material at the same time, and the antibacterial property of the silver-loaded material is obviously enhanced. The nano-silver-loaded composite material is simple and convenient in preparation process, low in requirement on a reaction device, mild in condition, green and environment-friendly, can be applied to large-scale production, and has good antibacterial performance.
Description
Technical Field
The invention belongs to the technical field of biological medicines, relates to a medical composite material carrying nano-silver, and particularly relates to a method for in-situ synthesis of nano-silver by a nanofiber or membrane carrier carrying a reductive plant extract and a method for preparing a nano-silver-carrying antibacterial composite material.
Background
With the overuse of antibiotics and the emergence of superbacteria, research is being directed to non-antibiotic antibacterials. Non-traditional antibacterial agents are capable of overcoming resistance caused by the use of antibiotics and are therefore subject to extensive research and attention. Among them, nano silver (AgNPs) is becoming a new generation of ideal antibacterial material due to its advantages of broad-spectrum antibacterial property, high efficiency, persistence, etc.
In the prior art, there are various methods for preparing silver nanoparticles. Although the reducing agent is adopted to reduce the silver precursor salt in the chemical method for preparing the nano silver, the used reducing agent has certain harmfulness, such as hydrazine, sodium borohydride and the like, and some by-products which are not environment-friendly can be generated. The physical method generally refers to preparing silver nanoparticles by methods such as a ball milling method, an arc discharge synthesis method and the like, the preparation method has large energy consumption and complex process, the obtained nanoparticles are easy to agglomerate, and the application of the method is limited to a certain extent; the nano silver prepared by the method has the defects of poor environmental protection property with different degrees, large energy consumption, multiple post-treatment processes of centrifugation, cleaning, dispersion and the like, and complicated steps.
If the silver-loaded medical composite material can be obtained while the nano silver is synthesized in a green way, the preparation process of the material is simplified and the industrial production is facilitated, so that the method for synthesizing and preparing the nano silver medical composite material with good antibacterial property and safety in a green, simple and rapid way is a popular subject in the research field.
Disclosure of Invention
In view of this, the invention provides a nano-silver-loaded antibacterial composite material and a preparation method thereof.
In order to achieve the above purpose, the invention provides the following technical scheme:
a nano-silver-loaded antibacterial composite material is prepared by adding a certain amount of reductive plant extract into a medical polymer material in the preparation process, directly placing the medical polymer material loaded with the reductive plant extract into a silver nitrate aqueous solution, and carrying out in-situ reduction synthesis to obtain the nano-silver-loaded antibacterial composite material.
Wherein the mass concentration of the reductive plant extract is 0.01-5%, and the reductive plant extract is curcumin or quercetin; and the grain diameter of the nano silver is 5-100nm.
In addition, the medical polymer material at least comprises one of polyvinyl alcohol, polycaprolactone, collagen, chitosan, silk fibroin, gelatin, sodium alginate, hyaluronic acid, polymethyl methacrylate, polylactic acid and polyvinylpyrrolidone.
The invention also provides a preparation method of the nano-silver-loaded antibacterial composite material, which comprises the following steps:
(a) Dissolving plant extract in medical polymer material solution to prepare blending solution; preparing the nanofiber or membrane carrier loaded with the plant extract under dark conditions by an electrostatic spinning technology, a freezing crosslinking method, a freeze-drying method or a casting method;
(b) Preparing a silver nitrate aqueous solution, and placing the nanofiber or membrane carrier loaded with the plant extract prepared in the step (a) in the silver nitrate aqueous solution to oscillate for a reduction reaction;
(c) And fully cleaning after the reduction reaction is completed to obtain the nano silver-loaded antibacterial composite material.
Preferably, in the step (a), the concentration of the medical polymer material solution is 1-20%.
Preferably, in the step (b), the concentration of the silver nitrate aqueous solution is 0.005-1M, the oscillation temperature is 15-40 ℃, and the reduction reaction time is 0.5-96h.
According to the technical scheme, compared with the prior art, the nano-silver-loaded antibacterial composite material and the preparation method thereof provided by the invention have the following excellent effects:
(1) The polymer medical material loaded with the reductive plant extract is used as a reactor, silver ions permeate into the material, and the silver-loaded medical composite material is prepared by green synthesis of nano silver through the reducibility of the plant extract, so that the raw materials are easily obtained, the cost is low, and the operation is convenient.
(2) The synthesis process does not need special conditions, can adjust the synthesis speed of the nano-silver by regulating and controlling the reaction time, the concentration of the reaction liquid, the reaction temperature and the like, has mild conditions, low energy consumption and short preparation period, and is a safe, high-efficiency, green and environment-friendly synthesis method.
(3) The reductive plant extract is used as a biological reducing agent to prepare the nano-silver, and the by-products are fewer. The silver-loaded composite material is obtained while the nano silver is synthesized in situ, multiple steps such as centrifugation, redispersion and the like are not needed, the preparation process is simplified, the silver nanoparticle loading rate is improved, the combination of the silver nanoparticles and the nano fiber or membrane material is firmer, the antibacterial capability of the silver-loaded composite material is effectively improved, and the silver-loaded composite material can be directly applied to medical purposes such as antibiosis and the like.
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 introduced below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a photograph of a curcumin-loaded PVA film and a nano silver-loaded composite film.
Fig. 2 is a color comparison graph of PVA films loaded with different curcumin contents placed in silver nitrate aqueous solutions with different concentrations.
FIG. 3 shows a PVA film material carrying curcumin and AgNO 3 Ultraviolet-visible spectrum of the reaction system after the aqueous solution reacts.
FIG. 4 is a scanning electron micrograph and an EDS signature.
FIG. 5 is a transmission electron micrograph of a silver-loaded composite.
FIG. 6 is a graph showing the results of the antibacterial activity test.
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 the accompanying drawings of the specification, 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.
The embodiment of the invention discloses a preparation method of a nano-silver-loaded antibacterial composite material.
In order to better understand the present invention, the following examples further specifically illustrate the present invention, but should not be understood as the definition of the invention, for those skilled in the art who have the above summary of the invention, some insubstantial modifications and adaptations are considered to fall within the scope of the invention.
The technical solution of the present invention will be further described with reference to the following specific examples.
Example 1
(1) Dissolving 1% of curcumin in acetic acid aqueous solution (10%, v/v) with PVA mass fraction of 8%, and mixing thoroughly;
(2) Preparing a curcumin-loaded PVA membrane by using 25% glutaraldehyde as a cross-linking agent through a freezing cross-linking method under a dark condition, and fully washing in purified water to remove residual glutaraldehyde;
(3) Preparing 0.01M silver nitrate aqueous solution; placing the curcumin-loaded PVA film carrier in a silver nitrate aqueous solution, placing the curcumin-loaded PVA film carrier in an oscillator under a dark condition, and reducing nano-silver in situ under the conditions that the temperature is 37 ℃ and the oscillation speed is 60rpm to obtain the silver-loaded PVA composite film at the same time.
The generation of nano silver is visually displayed by the color change of the material and the color change of a silver nitrate water solution (figures 1 and 2), wherein figure 1 (A) is a PCL nano fiber loaded with curcumin, (B) is a PCL nano fiber loaded with nano silver, (C) is a PVA film material loaded with curcumin, and (D) is a PVA medical film material loaded with nano silver;
and it can be seen from fig. 2 that the film color gradually deepens with the increase of the reaction time under the same silver nitrate concentration. In FIG. 2, the silver nitrate concentrations of A, B, C, D reaction solution were 0, 0.01M, 0.03M and 0.1M, respectively. The larger the silver nitrate concentration is at the same reaction time point, the darker the color of the obtained composite film carrying the nano silver is. The results prove that the synthesis rate of the nano silver can be adjusted by the reaction time and the concentration of the reaction solution.
In addition, the color of the polymer material loaded with curcumin is yellow, but the color of the material is changed and gradually deepened after the nano silver is successfully synthesized, and the silver-loaded material gradually becomes black (for example, the material is black when the nano silver powder is gathered together).
In FIG. 2, 0h is a picture that the reaction is not started just after adding the silver nitrate aqueous solution, and compared with the pictures of 0h, the film color is obviously deepened after reacting for 4h and reacting for 6h, which indicates that the nano silver is successfully synthesized; and 6h is the darkest, thereby indicating that the synthesis rate and the synthesis amount can be controlled by regulating and controlling the time.
And the comparison at the same time point (comparison of ABCD in the same figure) shows that D is the highest concentration of silver nitrate and the deepest color of the composite film, and proves that the nano-silver synthesis rate is higher and the synthesis amount is larger.
And the silver nitrate reaction solution has the change of the UV-Vis visible absorption peak. The curcumin-loaded PVA film is placed in silver nitrate aqueous solution to react for 1h at 37 ℃, the ultraviolet-visible spectrogram of the reaction system can obviously change, wherein the ultraviolet-visible spectrogram at 430nm is the SPR characteristic peak of the nano-silver, and the formation of the nano-silver is also confirmed from another angle (figure 3).
Example 2
(1) Dissolve 8% PCL in CHCl 3 Mixing with methanol solution, stirring, and standing overnight; dissolving 2% curcumin in PCL solution, stirring well and degassing for later use;
(2) By adopting an electrostatic spinning technology, parameters such as liquid pushing speed, spinning voltage, receiving distance and the like are adjusted, and PCL nano-fiber loaded with curcumin is prepared under a dark condition;
(3) Adding silver nitrate into deionized water to be fully dissolved, and preparing a silver nitrate water solution with the concentration of 0.1M;
(4) Placing PCL nano fiber loaded with curcumin in silver nitrate aqueous solution, placing in an oscillator under dark condition, adjusting the temperature to 30 ℃, adjusting the oscillation speed to 100rpm, reacting for 48h, reducing and synthesizing nano silver, and simultaneously obtaining the silver-loaded PCL composite nano fiber (figure 1).
Example 3
(1) Dissolving 5% of curcumin in a PVA acetic acid aqueous solution to prepare a blending solution;
(2) Preparing the nano-fiber or membrane carrier loaded with curcumin by an electrostatic spinning, freezing cross-linking or casting method under a dark condition;
(3) Adding weighed silver nitrate into deionized water for full dissolution to prepare 0.03M silver nitrate aqueous solution;
(4) Placing the curcumin-loaded nanofiber or membrane carrier in a silver nitrate aqueous solution, placing the curcumin-loaded nanofiber or membrane carrier in an oscillator under a dark condition, and reacting for 8 hours at the temperature of 20 ℃ to obtain the silver-loaded composite nanofiber or composite membrane.
The prepared silver-loaded composite material is fully cleaned and dried for later use, and the scanning electron microscope image shown in figure 4 shows that the surface particles of the silver-loaded PVA medical composite membrane material are nano silver, and EDS shows that the silver content is about 2.08%.
The transmission electron microscope shown in fig. 5 shows that the black particles are silver nanoparticles synthesized in situ on PCL fibers or PVA films; wherein, fig. 5 (a) is the PCL nanofiber loaded with nano silver, and fig. 5 (B) is the PVA medical membrane material loaded with nano silver.
Example 4
(1) Dissolving chitosan in 3% (v/v) acetic acid aqueous solution, stirring thoroughly and mixing uniformly to obtain chitosan solution with mass fraction of 6%, dissolving 2.5% (w/v) quercetin in chitosan solution, and ultrasonically mixing uniformly to remove bubbles for later use;
(2) Preparing a porous chitosan membrane carrier loaded with quercetin by a freeze-drying method;
(3) Adding silver nitrate into deionized water, and fully dissolving to obtain 0.1M silver nitrate water solution;
(4) And (3) placing the porous membrane loaded with the quercetin in a silver nitrate aqueous solution, placing the porous membrane in an oscillator under a dark condition, and carrying out in-situ reduction reaction for 24 hours at the temperature of 37 ℃ to obtain the nano-silver loaded chitosan composite material.
In addition, in order to further verify the antibacterial property of the nano silver-loaded composite material, the inventors also carried out the following experiment:
and respectively cutting the filter paper, the prepared PCL-CUR-Ag and PVA-CUR-Ag composite material for standby. Sterilizing nutrient agar culture medium, distributing into disposable sterile culture dish, and collecting 100ul of culture medium with concentration of 1x10 7 CFU/mL of the E.coli suspension was spread evenly on the surface of the solidified nutrient agar medium, and the test pieces were attached to the solid medium. Finally, the dish was placed in an incubator at a constant temperature and the photograph was taken after 24 hours of incubation at 37 ℃ as shown in FIG. 6. Inhibition zone existence certification systemThe prepared silver-loaded composite material has certain antibacterial capacity; wherein, fig. 6 (A) is filter paper, (B) is a silver-loaded PVA composite membrane, and (C) is silver-loaded PCL nano fiber.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. The nano-silver-loaded antibacterial composite material is characterized in that a certain amount of reductive plant extract is added in the preparation process of a medical high polymer material, the medical high polymer material loaded with the reductive plant extract is directly placed in a silver nitrate aqueous solution, and the nano-silver-loaded antibacterial composite material is obtained through in-situ reduction synthesis.
2. The nanosilver-loaded antibacterial composite material as claimed in claim 1, wherein the mass concentration of the reductive plant extract is 0.01% -5%, and the reductive plant extract is curcumin or quercetin.
3. The nanosilver-loaded antibacterial composite material of claim 1, wherein the medical polymer material comprises at least one of polyvinyl alcohol, polycaprolactone, collagen, chitosan, silk fibroin, gelatin, sodium alginate, hyaluronic acid, polymethyl methacrylate, polylactic acid, and polyvinylpyrrolidone.
4. The antibacterial composite material carrying nano silver as claimed in any one of claims 1 to 3, wherein the nano silver has a particle size of 5 to 100nm.
5. A method for preparing the antibacterial composite material carrying nano-silver as claimed in any one of claims 1 to 4, which is characterized by comprising the following steps:
(a) Dissolving plant extract in medical polymer material solution to prepare blending solution; preparing the nanofiber or membrane carrier loaded with the plant extract under dark conditions by an electrostatic spinning technology, a freezing crosslinking method, a freeze-drying method or a casting method;
(b) Preparing a silver nitrate aqueous solution, and placing the nanofiber or membrane carrier loaded with the plant extract prepared in the step (a) in the silver nitrate aqueous solution to oscillate for a reduction reaction;
(c) And fully cleaning after the reduction reaction is completed to obtain the nano silver-loaded antibacterial composite material.
6. The method for preparing the nano-silver-loaded antibacterial composite material as claimed in claim 5, wherein in the step (a), the concentration of the medical polymer material solution is 1-20%.
7. The method for preparing a nano-silver-loaded antibacterial composite material as claimed in claim 5, wherein in the step (b), the concentration of the silver nitrate aqueous solution is 0.005-1M, the oscillation temperature is 15-40 ℃, and the reduction reaction time is 0.5-96h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103705969A (en) * | 2014-01-02 | 2014-04-09 | 东华大学 | Method for preparing chitosan-based silver-loaded composite antimicrobial superfine fiber membrane |
| CN106880593A (en) * | 2017-02-21 | 2017-06-23 | 中国医学科学院放射医学研究所 | It is a kind of while nano antibacterial agent of loading nano silvery and curcumin and preparation method and application |
| CN114769611A (en) * | 2022-04-06 | 2022-07-22 | 电子科技大学中山学院 | Method for preparing nano-silver by utilizing pine needle extract |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103705969A (en) * | 2014-01-02 | 2014-04-09 | 东华大学 | Method for preparing chitosan-based silver-loaded composite antimicrobial superfine fiber membrane |
| CN106880593A (en) * | 2017-02-21 | 2017-06-23 | 中国医学科学院放射医学研究所 | It is a kind of while nano antibacterial agent of loading nano silvery and curcumin and preparation method and application |
| CN114769611A (en) * | 2022-04-06 | 2022-07-22 | 电子科技大学中山学院 | Method for preparing nano-silver by utilizing pine needle extract |
Non-Patent Citations (1)
| Title |
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| 姚平等: "前驱体浓度对槲皮素纳米银粒子制备及其催化性能的影响", 《印染》, no. 5, pages 26 - 31 * |
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