CN113070484A - Size-controllable spherical nano silver particles, preparation method and application - Google Patents
Size-controllable spherical nano silver particles, preparation method and application Download PDFInfo
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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Abstract
The invention belongs to the technical field of biological preparation of nano silver particles, and discloses a size-controllable spherical nano silver particle, a preparation method and application thereof, wherein the preparation method of the size-controllable spherical nano silver particle comprises the following steps: the silver nitrate solution is used as a silver source, the deionized water is used as a solvent, and the active component of the areca extract is used as a stabilizer and a reducing agent to prepare the nano silver colloid particles which have small particle size, regular spherical shape, good dispersibility and no agglomeration phenomenon. The preparation method of the spherical silver nanoparticles with controllable sizes comprises the following steps: extracting active ingredients of the waste areca nuts; and synthesizing spherical nano silver particles. The invention utilizes the extract of the waste areca nuts to synthesize the spherical nano-silver antibacterial particles with controllable size, stable shape and regularity. The nano silver particles prepared by the method have the advantages of small particle size, regular spherical shape, good dispersibility, no agglomeration phenomenon and stronger pathogenic bacteria resistance.
Description
Technical Field
The invention belongs to the technical field of biological preparation of nano silver particles, and particularly relates to a size-controllable spherical nano silver particle, a preparation method and application thereof.
Background
At present, metallic silver has a long history in the human development history as a traditional disinfectant. Compared with the metal silver with macroscopic size, the nano silver has unique physical and chemical properties, extremely large specific surface area and stronger sterilization performance. Moreover, the nano silver particles have very good biocompatibility, conductivity and biocatalysis performance, and thus have become the nano materials with the widest commercial application. So far, the nano silver particles have been used as antibacterial agents in the industries of medical treatment, food, textile, environmental protection, cosmetics, agricultural pest control and the like, and have been approved by the official scientific research institutions such as the U.S. FDA and EPA. At present, the synthesis methods of nano silver mainly comprise three methods: physical, chemical and biological methods. The traditional physical method has very high requirements on equipment and high production cost; the chemical synthesis method generally adopts a toxic organic solvent as a reducing agent, so that the pollution is serious, and the synthesized nano particles are easy to agglomerate; the nano silver particles prepared by the green, environment-friendly, mild and cheap biological synthesis method have regular shapes, smaller sizes, good stability and good biocompatibility. The waste betel nut fruit extract contains rich plant active components (polyphenol, flavone, polysaccharide and the like), and can be used as a reducing agent for synthesizing nano silver particles and a stabilizing agent thereof.
Through the above analysis, the problems and defects of the prior art are as follows: the existing synthesis method of the nano silver particles has very high requirements on equipment and high production cost; the pollution is serious, and the synthesized nano particles are easy to agglomerate; the biological preparation method has the advantages of simple and rapid synthesis, small size of the obtained nano silver ions, good stability, strong bacteriostatic ability and the like. Solves the scientific problems of high cost, large pollution, large particle size, poor stability, easy agglomeration and the like of the nano silver particles synthesized by the traditional method.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a size-controllable spherical nano silver particle, a preparation method and application thereof.
The invention is realized in such a way that the size-controllable spherical nano silver particles, the preparation method and the application thereof are disclosed, and the preparation method of the size-controllable spherical nano silver particles comprises the following steps: the silver nitrate solution is used as a silver source, the deionized water is used as a solvent, and the active component of the areca extract is used as a stabilizer and a reducing agent to prepare the nano silver colloid particles which have small particle size, regular spherical shape, good dispersibility and no agglomeration phenomenon.
Further, the preparation method of the spherical silver nanoparticles with controllable size comprises the following steps:
step one, extracting active ingredients of waste areca nuts;
and step two, synthesizing the spherical nano silver particles.
Further, in the first step, the extracting of the active ingredients of the waste areca nuts comprises: collecting fresh areca nut kernels, and cleaning the areca nut kernels with deionized water; after freeze-drying, pulverizing and sieving with 40 mesh sieve by a pulverizer for later use. Mixing 20g of the areca nut kernel powder with 200mL of deionized water uniformly, carrying out water bath for 1.5h at 90 ℃, then centrifuging and filtering, and taking supernatant, namely the areca nut kernel extracting solution.
Further, in the second step, the synthesizing of the spherical silver nanoparticles includes:
adding the extracted areca nut kernel water extract into 0-1.0 mM silver nitrate solution, adjusting the pH value of the mixed solution to 2-12, and uniformly mixing and stirring for 5-120 min;
further, in the step (1), the concentration of the areca seed kernel water extract is 1 mg/mL.
The invention also aims to provide the spherical silver nanoparticles with controllable size prepared by the method. Further, when the areca nut kernel water extract reacts with 1.0mM silver nitrate solution; when the pH value is 12 and the reaction time is 90min, the nano silver particles with the minimum particle size can be obtained. The size of the nano silver particles is 4-10 nm.
The invention further aims to provide application of the spherical silver nanoparticles with controllable sizes in inhibiting pathogenic bacteria.
The invention also aims to provide application of the spherical silver nanoparticles with controllable sizes in the aspect of antioxidation in the field of cosmetics.
By combining all the technical schemes, the invention has the advantages and positive effects that: the invention utilizes the extract of the waste areca nuts to synthesize the spherical nano-silver antibacterial particles with controllable size, stable shape and regularity. The nano silver particles prepared by the method have the advantages of small particle size, regular spherical shape, good dispersibility, no agglomeration phenomenon and stronger oxidation resistance and pathogenic bacteria resistance.
The method takes silver nitrate solution as a silver source, deionized water as a solvent and active ingredients (polyphenol, polysaccharide and the like) of areca extract as a stabilizer and a reducing agent, and nano silver colloid particles which are small in size, stable in shape and regular in spherical shape are rapidly prepared in a green way. The method has the advantages of simple process, rapid and mild reaction, environmental protection and the like. Moreover, the nano silver particles synthesized by the method have broad spectrum and strong capability of inhibiting pathogenic bacteria. The spherical nano silver particles have very great application prospect in the fields of food packaging, cosmetics and pathogenic microorganism prevention and control.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
Fig. 1 is a flow chart of a size-controllable spherical silver nanoparticle and a preparation method thereof provided by the embodiment of the invention.
Fig. 2 is a schematic diagram illustrating the influence of the reaction time on the color of the silver nanoparticles, the ultraviolet spectral characteristics and the particle size according to the embodiment of the present invention.
Fig. 3 is a schematic diagram illustrating the influence of silver nitrate concentration on the color and ultraviolet spectrum characteristics of nano-silver particles and the particle size according to an embodiment of the present invention.
Fig. 4 is a schematic diagram illustrating the influence of the reaction pH on the color and ultraviolet spectrum characteristics of the silver nanoparticles and the particle size according to an embodiment of the present invention.
Fig. 5 is a schematic electron microscope diagram of the silver nanoparticles in the optimal reaction system provided by the embodiment of the invention.
Fig. 6 is a schematic diagram of the stability of the silver nanoparticles under the optimal reaction system provided by the embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a size-controllable spherical nano silver particle, a preparation method and application thereof, and the invention is described in detail below with reference to the accompanying drawings.
The preparation method of the spherical silver nanoparticles with controllable sizes, provided by the embodiment of the invention, comprises the following steps:
the silver nitrate solution is used as a silver source, the deionized water is used as a solvent, and the active component of the areca extract is used as a stabilizer and a reducing agent to prepare the nano silver colloid particles which have small particle size, regular spherical shape, good dispersibility and no agglomeration phenomenon.
As shown in fig. 1, the preparation method of the size-controllable spherical silver nanoparticles provided by the embodiment of the present invention includes the following steps:
s101, extracting active ingredients of areca nut kernels;
and S102, synthesizing spherical nano silver particles.
In step S101, the extracting of the active ingredient of the waste betel nut provided by the embodiment of the present invention includes: collecting fresh areca nuts, and cleaning the areca nuts with deionized water; after drying, the mixture is crushed by a pulverizer and sieved by a 40-mesh sieve for later use. Mixing 20g of the areca nut kernel powder with 200mL of deionized water uniformly, carrying out water bath for 1.5h at 90 ℃, then centrifuging and filtering, and taking supernatant, namely the areca nut kernel extracting solution.
In step S102, the synthesizing of the spherical silver nanoparticles provided in the embodiment of the present invention includes:
(1) adding the extracted areca nut kernel extracting solution into 0-1.0 mM silver nitrate solution, adjusting the pH value of the mixed solution to 2-12, and mixing and stirring uniformly;
(2) and (3) placing the silver particles in ultrasonic waves for ultrasonic treatment to obtain the nano silver particles with controllable size, stable shape and regular spherical shape.
In the step (1), the concentration of the areca nut kernel extract provided by the embodiment of the invention is 1 mg/mL.
In step (2), the ultrasonic treatment provided by the embodiment of the present invention includes: ultrasonic treatment is carried out for 5 min-2 h at the temperature of 30 ℃ under the condition of 300W.
The size of the nano silver particles provided by the embodiment of the invention is 4-10 nm.
The technical effects of the present invention will be further described with reference to specific embodiments.
Example 1:
the invention relates to size-controllable nano-silver antibacterial particles and a preparation method and application thereof, and the size-controllable nano-silver antibacterial particles comprise the following steps:
(1) preparing an areca seed kernel extracting solution: collecting fresh areca nuts, and cleaning the areca nuts with deionized water;
(2) synthesizing spherical nano silver particles;
(3) observing and characterizing the form of the nano silver particles;
(4) and (4) determining the bacteriostatic ability of the nano silver particles.
Based on the scheme, the method takes silver nitrate solution as a silver source, deionized water as a solvent and active ingredients (polyphenol, polysaccharide and the like) of areca extract as a stabilizer and a reducing agent, and nano silver colloid particles which are small in size, stable in form and regular in spherical shape are rapidly prepared in a green mode. The method has the advantages of simple process, rapid and mild reaction, environmental protection and the like. Moreover, the synthesized nano silver particles have broad spectrum and strong capability of inhibiting pathogenic bacteria. The spherical nano silver particles have great application prospect in the fields of food packaging, cosmetics and prevention and treatment of tropical crop pathogenic bacteria.
The detection data of the silver nanoparticles of the present invention are shown in table 1.
TABLE 1 inhibitory Effect of the synthesized silver nanoparticles on common pathogenic bacteria
According to the method, active ingredients of the waste areca nuts are extracted by deionized water, a waste areca nut water extract (1mg/mL) with a proper concentration is added into a 0-1.0 mM silver nitrate solution, the pH value (2-12) of a mixed solution is adjusted, the mixed solution is uniformly mixed and stirred, the mixed solution is placed in ultrasonic waves and subjected to ultrasonic treatment at 30 ℃ for 5 min-2 h, and then the nano silver particles (4-10 nm) with controllable size, stable shape and regular spherical shape can be obtained. The method takes silver nitrate solution as a silver source, deionized water as a solvent and active ingredients (polyphenol, polysaccharide and the like) of areca nut kernel extract as a stabilizer and a reducing agent, and the nano silver colloid particles which are small in particle size, regular in spherical shape, good in dispersity and free of agglomeration are rapidly prepared in a green mode. The method has the advantages of simple process, rapid and mild reaction, environmental protection and the like. Moreover, the synthesized nano silver particles have broad spectrum and strong capability of inhibiting pathogenic bacteria. The spherical nano silver particles have very great application prospect in the fields of cosmetics, textile industry and pathogenic microorganism prevention and control.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of spherical silver nanoparticles with controllable size is characterized by comprising the following steps: the silver nitrate solution is used as a silver source, the deionized water is used as a solvent, and the active component of the areca extract is used as a stabilizer and a reducing agent to prepare the nano silver colloid particles which have small particle size, regular spherical shape, good dispersibility and no agglomeration phenomenon.
2. The method of preparing spherical silver nanoparticles with controllable size according to claim 1, wherein the method of preparing spherical silver nanoparticles with controllable size comprises the following steps:
step one, extracting active ingredients of waste areca nuts;
and step two, synthesizing the spherical nano silver particles.
3. The method for preparing spherical silver nanoparticles with controllable size according to claim 2, wherein the extracting active components from the betel nut kernels in the first step comprises: collecting fresh areca nuts, and cleaning the areca nuts with deionized water; after freeze-drying, pulverizing and sieving with 40 mesh sieve by a pulverizer for later use. Mixing 20g of the areca nut kernel powder with 200mL of deionized water uniformly, carrying out water bath for 1.5h at 90 ℃, then centrifuging and filtering, and taking supernatant, namely the areca nut kernel extracting solution.
4. The method according to claim 2, wherein the step two, the synthesizing of the spherical silver nanoparticles comprises: adding the extracted water extract of the waste areca nuts into 0-1.0 mM silver nitrate solution, adjusting the pH value of the mixed solution to 2-12, mixing and stirring uniformly, and reacting for 0-120min to obtain the regular spherical nano silver particles with controllable size and stable shape.
5. The method of claim 4, wherein the concentration of the extract solution of areca nut kernel is 1 mg/mL.
6. The method for preparing the size-controllable spherical silver nanoparticles according to claim 4, wherein the optimal scheme is as follows: the silver nitrate solution was 1.0mM, pH 12, and reaction time 90 min.
7. Size-controllable spherical silver nanoparticles prepared by the method for preparing silver nanoparticles according to any one of claims 1 to 6.
8. The size-controllable spherical silver nanoparticles according to claim 1, wherein the size of the silver nanoparticles is 4 to 10 nm.
9. Use of the size-controllable spherical silver nanoparticles according to claim 7 for inhibiting pathogenic microorganisms.
10. Use of the spherical silver nanoparticles with controllable size according to claim 7 in the cosmetic antioxidation field.
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