CN112426982A - Rapid preparation method of silver-based magnetic nano-microspheres - Google Patents
Rapid preparation method of silver-based magnetic nano-microspheres Download PDFInfo
- Publication number
- CN112426982A CN112426982A CN202011298366.3A CN202011298366A CN112426982A CN 112426982 A CN112426982 A CN 112426982A CN 202011298366 A CN202011298366 A CN 202011298366A CN 112426982 A CN112426982 A CN 112426982A
- Authority
- CN
- China
- Prior art keywords
- silver
- microspheres
- magnetic
- based magnetic
- nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
Abstract
The invention discloses a rapid preparation method of silver-based magnetic nano microspheres, which relates to the technical field of silver-based nano material preparation, and comprises the following steps: dispersing the pretreated magnetic nano-microspheres in an alkaline buffer solution; adding silver nitrate powder into the solution, and stirring for reaction under ultraviolet irradiation; separating the product obtained by stirring reaction under the action of a magnetic field to obtain a solid product; and removing impurities from the solid product and drying to obtain the silver-based magnetic nano-microspheres. The method has mild reaction conditions, and does not need additional reducing agent; the surface groups of the magnetic nano-microspheres are activated by ultraviolet light, and the silver nano-particles are reduced to be deposited on the surfaces of the magnetic nano-microspheres, so that the reaction time is effectively shortened, the dispersibility of the silver nano-particles is improved, and the chemical activity of the silver-based magnetic nano-microspheres is improved.
Description
Technical Field
The invention relates to the technical field of silver-based nano material preparation, in particular to a preparation method of silver-based magnetic nano microspheres.
Background art:
the nano-sized silver material has been widely studied by researchers due to its excellent physical and chemical properties. According to the characteristics of the materials, the materials with different properties are prepared, so that the silver nanoparticles can be widely used as a sterilization material, a catalyst, an energy storage material, a sensor, a medical material and an SERS substrate. In recent years, the compounding of silver nano materials and other functional materials attracts people's extensive attention, and the silver-based nano composite materials have further application.
At present, there are many methods for preparing silver nano-materials, such as hydrothermal method, precipitation method, sol-gel method, and interfacial synthesis method. However, due to the high specific surface ratio of silver itself, the small size and the high surface energy generated by surface defects, the above preparation method often causes particle agglomeration, thereby reducing its own activity. Therefore, the silver nanoparticles are loaded on other functional materials, such as graphene materials, semiconductor materials, conductive polymer materials, magnetic materials and the like, but the defects of overlong preparation time and the like still need to be overcome.
Disclosure of Invention
The invention aims to provide a rapid preparation method of silver-based magnetic nano microspheres, which aims to overcome the defect that the time for preparing the silver-based magnetic nano microspheres is too long in the prior art.
A method for rapidly preparing silver-based magnetic nano microspheres comprises the following steps:
s1, dispersing the pretreated magnetic nano-microspheres in an alkaline buffer solution;
s2, adding silver nitrate powder into the S1 solution, and stirring to react under ultraviolet irradiation;
s3, separating the product obtained by the stirring reaction in the step S2 under the action of a magnetic field to obtain a solid product;
and S4, removing impurities from the solid product obtained in the step S3, and drying to obtain the required silver-based magnetic nano microspheres.
Further, in step S1, the method for pre-treating the magnetic nanospheres includes wrapping the magnetic nanoparticles with Polydopamine (PDA).
Further, in step S2, the mass ratio of the magnetic nanoparticles to the silver nitrate when the silver-based magnetic nanoparticles are obtained by the reduction reaction is 1:1 to 1: 3.
Further, in step S1, the magnetic nanoparticles include at least one of: alloy nanoparticles, ferrite nanoparticles, and intermetallic compound nanoparticles.
Further, in step S2, the stirring reaction is performed under ultraviolet irradiation for 20 to 40 minutes.
Further, in step S4, the method for removing impurities from the solid product includes:
the product obtained from the magnetic separation in step S3 was washed alternately with water and ethanol at least 6 times.
The invention has the advantages that: the preparation method of the silver-based magnetic nano-microsphere comprises the following steps:
(1) the reaction conditions are mild, and the silver-based magnetic nano-microspheres can be obtained by a one-step method;
(2) the invention accelerates the reaction process and greatly shortens the preparation time of the silver-based magnetic nano-microspheres by adopting ultraviolet irradiation for 20-40 minutes.
Drawings
Fig. 1 is a schematic diagram of the preparation of the silver-based magnetic nanospheres of the present invention.
FIG. 2 is a transmission electron microscope image of the silver-based magnetic nanospheres of the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Fe is selected as the magnetic nanoparticles in the following examples3O4For the alkaline buffer, a Tris buffer solution with a pH of 8.5 is used for the description.
As shown in fig. 1 to 2, a method for preparing silver-based magnetic nanospheres comprises the following steps:
dispersing the pretreated magnetic nano-microspheres in an alkaline buffer solution;
adding silver nitrate powder into the solution, and stirring for reaction under ultraviolet irradiation;
separating the product obtained by stirring reaction under the action of a magnetic field to obtain a solid product;
and removing impurities from the solid product and drying to obtain the silver-based magnetic nano-microspheres.
In this embodiment, the method for pretreating the magnetic nanospheres comprises coating the magnetic nanoparticles with polydopamine.
In this embodiment, the mass ratio of the magnetic nanospheres to the silver nitrate when the silver-based magnetic nanospheres are obtained by a reduction reaction is 1:1-1: 3.
in this embodiment, the magnetic nanoparticles comprise at least one of: alloy nanoparticles, ferrite nanoparticles, and intermetallic compound nanoparticles.
In this example, the stirring reaction condition is ultraviolet irradiation for 20 to 40 minutes.
In this embodiment, the method for removing impurities from the solid product includes:
performing magnetic separation on a product obtained by the mixing reaction;
the solid product was washed at least 6 times with water and ethanol.
The process of the invention is further illustrated by the following examples:
example 1
According to Fe respectively3O4The mass ratio of @ PDA to silver nitrate is 1:1, 1:2, 1:3, and Fe is functionalized3O4@ PDA was ultrasonically dispersed in Tris buffer at 50ml pH 8.5, and a certain amount of silver nitrate was added thereto, followed by reaction under stirring under ultraviolet irradiation for 30 minutes. And after the reaction is finished, separating by using an external magnetic field to obtain a solid product, repeatedly washing by using water and ethanol to remove impurities, and drying to obtain the required silver-based magnetic nano-microspheres.
Example 2
According to Fe3O4The mass ratio of @ PDA to silver nitrate is 1:2, and Fe is functionalized3O4And ultrasonically dispersing the @ PDA in a Tris buffer solution with the pH value of 50 mlL being 8.5, adding a certain amount of silver nitrate, and stirring to react for 20, 30 and 40 minutes under ultraviolet irradiation. After the reaction is finished, separating by using an external magnetic field to obtain a solid product, repeatedly washing by using water and ethanol to remove impurities,drying to obtain the silver-based magnetic nano-microspheres.
Based on the above, the specific gravity of the magnetic nanoparticles and silver nitrate is 1:2, the reaction time under ultraviolet irradiation is 30 minutes, compared with the conventional preparation conditions, the preparation time of the silver-based magnetic nanoparticles is greatly shortened, and meanwhile, the dispersibility and the chemical activity are improved.
Reference is made to Pan X, Cheng S, Su T, et al Poly (2-hydroxyphenyl amines) functional magnetic polypopamine nanoparticles for high-efficiency DNA isolation applied Surface Science 2019,498: 143888.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Claims (6)
1. A rapid preparation method of silver-based magnetic nano-microspheres is characterized by comprising the following steps:
s1, dispersing the pretreated magnetic nano-microspheres in an alkaline buffer solution;
s2, adding silver nitrate powder into the solution obtained in the step S1, and stirring and reacting under ultraviolet irradiation to obtain a stirred product;
s3, separating the product obtained by the stirring reaction in the step S2 under the action of a magnetic field to obtain a solid product;
and S4, removing impurities from the solid product obtained in the step S3, and drying to obtain the required silver-based magnetic nano microspheres.
2. The method for rapidly preparing the silver-based magnetic nanospheres according to claim 1, wherein the method comprises the following steps: in step S1, the method for pre-treating the magnetic nanoparticle includes wrapping the magnetic nanoparticle with polydopamine.
3. The method for rapidly preparing the silver-based magnetic nanospheres according to claim 1, wherein the method comprises the following steps: in step S2, when the silver-based magnetic nanospheres are obtained by a reduction reaction, the mass ratio of the magnetic nanospheres to the silver nitrate is 1:1-1: 3.
4. The method for rapidly preparing the silver-based magnetic nanospheres according to claim 1, wherein the method comprises the following steps: in step S1, the magnetic nanoparticles include at least one of: alloy nanoparticles, ferrite nanoparticles, and intermetallic compound nanoparticles.
5. The method for rapidly preparing the silver-based magnetic nanospheres according to claim 1, wherein the method comprises the following steps: in step S2, the stirring reaction under ultraviolet irradiation is performed under conditions of ultraviolet irradiation for 20 to 40 minutes while performing the stirring reaction.
6. The method for rapidly preparing the silver-based magnetic nanospheres according to claim 1, wherein the method comprises the following steps: in step S4, the method of removing impurities from the solid product includes:
and (5) alternately washing the product obtained after the magnetic separation in the step S3 for at least 6 times by water and ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011298366.3A CN112426982A (en) | 2020-11-19 | 2020-11-19 | Rapid preparation method of silver-based magnetic nano-microspheres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011298366.3A CN112426982A (en) | 2020-11-19 | 2020-11-19 | Rapid preparation method of silver-based magnetic nano-microspheres |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112426982A true CN112426982A (en) | 2021-03-02 |
Family
ID=74694290
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011298366.3A Pending CN112426982A (en) | 2020-11-19 | 2020-11-19 | Rapid preparation method of silver-based magnetic nano-microspheres |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112426982A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1973908A (en) * | 2006-12-11 | 2007-06-06 | 张国栋 | Air purifying column of active carbon supported Ag and TiO2 photocatalyst for indoor air purifier |
| WO2013103322A1 (en) * | 2012-01-05 | 2013-07-11 | Nanyang Technological University | Methods of preparing monodispersed polydopamine nano- or microspheres, and methods of preparing nano-or microstructures based on the polydopamine nano- or microspheres |
| CN107442178A (en) * | 2017-08-02 | 2017-12-08 | 浙江理工大学 | A kind of visible light catalyst Fe3O4The preparation method of@PDA@Ag complex microspheres |
| CN110559471A (en) * | 2019-08-06 | 2019-12-13 | 中山大学 | Embolism microsphere with developing function and UCST responsiveness and preparation method thereof |
-
2020
- 2020-11-19 CN CN202011298366.3A patent/CN112426982A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1973908A (en) * | 2006-12-11 | 2007-06-06 | 张国栋 | Air purifying column of active carbon supported Ag and TiO2 photocatalyst for indoor air purifier |
| WO2013103322A1 (en) * | 2012-01-05 | 2013-07-11 | Nanyang Technological University | Methods of preparing monodispersed polydopamine nano- or microspheres, and methods of preparing nano-or microstructures based on the polydopamine nano- or microspheres |
| CN107442178A (en) * | 2017-08-02 | 2017-12-08 | 浙江理工大学 | A kind of visible light catalyst Fe3O4The preparation method of@PDA@Ag complex microspheres |
| CN110559471A (en) * | 2019-08-06 | 2019-12-13 | 中山大学 | Embolism microsphere with developing function and UCST responsiveness and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9446953B2 (en) | Fabrication of metallic hollow nanoparticles | |
| US8529963B2 (en) | Method for preparing dispersions of precious metal nanoparticles and for isolating such nanoparticles from said dispersions | |
| CN106670501B (en) | Preparation method of graphene-metal matrix composite powder | |
| KR101091416B1 (en) | Method for preparing radioisotope nanoparticle with core-shell structure and radioisotope nanoparticle thereby | |
| US20110262646A1 (en) | Surfactant-Assisted Inorganic Nanoparticle Deposition on a Cellulose Nanocrystals | |
| JP2013541640A (en) | Silver particles and method for producing the same | |
| WO2006082962A1 (en) | Method for producing composite particles | |
| CN106323935B (en) | Magnetic composite SERS substrate with core-shell-satellite three-dimensional structure and preparation method thereof | |
| CN113369491B (en) | Spherical and flaky mixed silver powder and manufacturing method thereof | |
| JP2009235474A (en) | Method for producing silver powder | |
| Yang et al. | Preparation of oleic acid-capped copper nanoparticles | |
| Lin et al. | In situ synthesis of easily separable Au nanoparticles catalysts based on cellulose hydrogels | |
| CN112624096A (en) | Graphene surface dispersibility modification method | |
| KR101890463B1 (en) | Method for fabricating hollow metal nano particles and hollow metal nano particles fabricated by the method | |
| CN112426982A (en) | Rapid preparation method of silver-based magnetic nano-microspheres | |
| CN107383725A (en) | A kind of preparation method of gadolinium metal organic frame/polyvinyl alcohol nano composite membrane | |
| CN105209660A (en) | Method for coating of carbon nanomaterials | |
| Jiang et al. | Preparation of silver quantum dots embedded water-soluble silica/PAAc hybrid nanoparticles and their bactericidal activity | |
| CN103071788A (en) | Method of preparing nickel-silver nuclear shell structure nano-particles | |
| KR101438505B1 (en) | Composite having zero valent iron, lipids and alginate and method for fabricating the same | |
| CN112041266A (en) | Method for obtaining nano material composed of carbon-containing material and metal oxide | |
| CN113817179B (en) | Preparation method of nanofiber magnetic fluid, nanofiber magnetic fluid and application | |
| CN108500292A (en) | A kind of preparation method of chain-like metal Ni nanopowders | |
| KR101375869B1 (en) | Chemically Converted Graphene Nano-composite Decorated with Dendrimer-encapsulated Nanoparticles and Method for Preparing the Same | |
| CN110681860B (en) | Graphene oxide coated metal composite nano with Raman signal and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |