CN110732680A - Method for preparing silver nano particles by using aminated column [5] arene as stabilizer - Google Patents

Method for preparing silver nano particles by using aminated column [5] arene as stabilizer Download PDF

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Publication number
CN110732680A
CN110732680A CN201911178620.3A CN201911178620A CN110732680A CN 110732680 A CN110732680 A CN 110732680A CN 201911178620 A CN201911178620 A CN 201911178620A CN 110732680 A CN110732680 A CN 110732680A
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solution
column
arene
aminated
amination
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孙燕
崔玉荃
吴若
郭放
郇文慧
刁国旺
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Yangzhou University
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Yangzhou University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/065Spherical particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102Metallic powder coated with organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B22F2009/245Reduction reaction in an Ionic Liquid [IL]

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses amination columns [5]]The method for preparing the silver nano particles by taking the aromatic hydrocarbon as the stabilizer comprises the following steps: column [5] aminated]Adding AgNO into aromatic solution3The solution is quickly stirred, and NaBH is quickly injected into the solution4Stirring the solution for 5-10 minutes to obtain an amination column [5]]Arene-protected silver nanoparticles. The method solves the defects that impurities are easy to generate and the structure of the silver nanoparticles is easy to damage in the traditional preparation method, and enough binding sites can include small organic molecules.

Description

Method for preparing silver nano particles by using aminated column [5] arene as stabilizer
Technical Field
The invention belongs to the technical field of nano materials, and relates to a preparation method of silver nano particles.
Background
Because of its many unique properties, such as surface and interface effect, small size effect, tunneling effect, quantum size effect, is attracting the attention of scientists, and because of these unique properties, silver nano-materials have -wide application in electric, acoustic, optical, catalytic and other fields.
Although researchers have conducted various researches and obtained definite results, silver-based antibacterial agents are difficult to realize industrial production due to experimental conditions and cost limitations, and the existing preparation methods often ignore the influences of toxicity of raw materials and solvents on organisms and environment.
Disclosure of Invention
The invention aims to provide methods for preparing silver nanoparticles by using amination column [5] arene as a stabilizer.
The technical proposal for realizing the aim of the invention is that methods for preparing silver nano particles by taking amination column [5] arene as a stabilizer comprise the following steps:
1) preparing an amination column [5] arene solution with the pH = 0.5-2.0;
2) AgNO with the preparation concentration of 9.7mM3A solution;
3) column [5] aminated]Adding AgNO into aromatic solution3The solution is stirred rapidly at the stirring speed of 350-500 r/min for 5-10 minutes, and NaBH with the concentration of 0.01-0.20M is injected into the solution rapidly4Stirring the solution for 5-10 min to change the color of the solution and turn the solution into bright yellow to obtain the aminated column [5]]Arene-protected silver nanoparticles.
Preferably, an amination column [5]]Aromatic hydrocarbons and AgNO3In a molar ratio of 1: 20-1: 50.
preferably, NaBH4With AgNO3In a molar ratio of 1: 10-1: 1: 100.
compared with the prior art, the invention has the advantages that:
1) the amination column [5] arene is used as a stabilizer to prepare the silver nanoparticles, and the reagent has the advantages of good dispersibility, strong stability, simple and convenient operation and time saving in the preparation of the silver nanoparticles.
2) The amido column [5] arene is non-toxic and harmless, is modified around the silver nanoparticles, and provides a wider space for the application of the silver nanoparticles.
Drawings
FIG. 1 shows that NaBH is added when Ag nanoparticles are prepared according to the invention4The TEM photograph thereafter.
FIG. 2 is a distribution diagram of the particle size of Ag nanoparticles prepared by the present invention.
FIG. 3 shows that NaBH with different concentrations is added during the preparation of Ag nanoparticles4Ultraviolet ray after irradiation.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in detail below with reference to examples.
The method for preparing the silver nanoparticles by using the aminated column [5] arene as the stabilizer obtains good use results, combines the column arene and the nano silver, is equivalent to the combination of supermolecule and nano materials, can well play the advantages and the performances of the column arene and the nano silver, and has great space for the further research of step .
The molecular structural formula of the amination-modified column [5] arene is as follows:
Figure 858532DEST_PATH_IMAGE002
example 1
(1) preparation of amination column [5] arene solution at pH = 1.0: 2.6 mg of aminated column [5] arene was weighed into dilute nitric acid pH =1.0 and stirred for 5 min.
(2) Amination column [5]Preparing silver nanoparticles by using arene as a stabilizer: to the above 8mL amination column [5]]Adding 9.7 mmoL of AgNO into aromatic hydrocarbon solution3Rapidly stirring for 5 minutes at the rotating speed of 350-plus-material 500 r/min, and then respectively and rapidly injecting the freshly prepared NaBH4(0.01 M) The solution was stirred for 5 minutes at 0.8mL, and the color of the solution was observed to change to bright yellow.
Example 2
(1) preparation of amination column [5] arene solution at pH = 1.0: 5.2 mg of aminated column [5] arene was weighed into an aqueous solution adjusted to pH =1.0 with concentrated nitric acid and stirred for 5 min.
(2) Amination column [5]Preparing silver nanoparticles by using arene as a stabilizer: to a prepared 8mL amination column [5]]Adding 9.7 mmoL of AgNO into aromatic hydrocarbon solution3Quickly stirring for 5min, and respectively and quickly injecting newly prepared NaBH4(0.20M) 1 mL of the solution was stirred for 10 minutes to observe the change in color of the solution.
As shown in FIG. 1, the silver nanoparticles prepared by the invention have good dispersibility and are in a nano-sphere shape.
FIG. 2 is a statistical graph of the particle size distribution of the silver nanoparticles prepared according to the present invention, wherein the particle size distribution of the nanoparticles prepared according to the present invention is in the range of 1-11 nm. Most of them are around 5.7 nm.
FIG. 3 is an ultraviolet absorption spectrum of silver nanoparticles prepared by the present invention, the maximum absorption peak is about 420 nm, which is the ultraviolet characteristic peak of the silver nanoparticles.

Claims (8)

1, amination columns [5]]The method for preparing the silver nano particles by taking the aromatic hydrocarbon as the stabilizer is characterized by comprising the following steps: column [5] aminated]Adding AgNO into aromatic solution3The solution is quickly stirred, and NaBH is quickly injected into the solution4And stirring the solution for 5-10 minutes.
2. The method of claim 1, wherein the pH of the aminated column [5] arene solution is = 0.5-2.0.
3. The method of claim 1, wherein the concentration of the amination column [5] arene solution is 0.6 to 0.75 mg/mL.
4. The method of claim 1, wherein AgNO3The concentration of the solution was 9.7 mM.
5. The method as claimed in claim 1, wherein the stirring speed of the rapid stirring is 350-500 r/min for 5-10 min.
6. The method of claim 1, wherein the NaBH is4The concentration of the solution is 0.01-0.20M.
7. The method of claim 1, wherein the column [5] is aminated]Aromatic hydrocarbons and AgNO3In a molar ratio of 1: 20-1: 50.
8. the method of claim 1, wherein the NaBH is4With AgNO3In a molar ratio of 1: 10-1: 100.
CN201911178620.3A 2019-11-27 2019-11-27 Method for preparing silver nano particles by using aminated column [5] arene as stabilizer Pending CN110732680A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114085298A (en) * 2021-11-30 2022-02-25 扬州大学 Water-soluble supramolecular inclusion compound DPG and preparation method and application thereof

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WO2015166253A1 (en) * 2014-05-02 2015-11-05 University Of Warwick Nanocrystals
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KR20120077308A (en) * 2010-12-30 2012-07-10 고려대학교 산학협력단 Preparation method for metal nanoparticles using glyme
WO2015166253A1 (en) * 2014-05-02 2015-11-05 University Of Warwick Nanocrystals
CN104447363A (en) * 2014-11-11 2015-03-25 西北师范大学 Cationic water-soluble column [5] aromatic hydrocarbon and preparation thereof and application of cationic water-soluble column [5] aromatic hydrocarbon in silver ion detection serving as acceptor
CN107486240A (en) * 2017-05-19 2017-12-19 中国科学院兰州化学物理研究所 A kind of ionic liquid cross-linked polymer load Technique of Nano Pd metal catalytic material and preparation method and application
CN107755710A (en) * 2017-10-17 2018-03-06 西南林业大学 A kind of method for preparing gold nano grain
CN109698335A (en) * 2018-12-19 2019-04-30 扬州大学 A kind of preparation method of column [5] aromatic hydrocarbons composite sulfur lithium sulphur positive electrode

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JING SUN等: "Electrochemical detection of paraquat based on silver nanoparticles/water-soluble pillar[5]arene functionalized graphene oxide modified glassy carbon electrode", 《JOURNAL OF ELECTROANALYTICAL CHEMISTRY》 *
JUN ZHOU等: "Synergistically Enhanced Electrochemical Response of Host−Guest Recognition Based on Ternary Nanocomposites: Reduced Graphene Oxide-Amphiphilic Pillar[5]arene-Gold Nanoparticles", 《ACS APPLIED MATERIALS & INTERFACES》 *
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114085298A (en) * 2021-11-30 2022-02-25 扬州大学 Water-soluble supramolecular inclusion compound DPG and preparation method and application thereof
CN114085298B (en) * 2021-11-30 2022-09-16 扬州大学 Water-soluble supramolecular inclusion compound DPG and preparation method and application thereof

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Application publication date: 20200131