CN103464782A

CN103464782A - Method utilizing shaddock ped extracting solution to synthesize silver nanoparticles in microwave

Info

Publication number: CN103464782A
Application number: CN2013104187597A
Authority: CN
Inventors: 张元�; 陈敏; 姜德立; 徐露璐; 吴柱东
Original assignee: Jiangsu University
Current assignee: Jiangsu University
Priority date: 2013-09-16
Filing date: 2013-09-16
Publication date: 2013-12-25

Abstract

The invention relates to a preparation method of silver nanoparticles, in particular to a method utilizing shaddock ped extracting solution to synthesize silver nanoparticles in microwave. The preparation method includes preparing the prepared shaddock ped extracting solution to volume, mixing and stirring the prepared shaddock ped extracting solution with silver nitrate solution in a certain concentration after a certain period of time, transferring the mixture to a microwave reactor, reacting for a while under a certain power, performing centrifugal separation to products, and washing the products with deionized water and ethyl alcohol many times to acquire collargol silver nanoparticles. The preparation method is green and environmental protective, and convenient and efficient, and grain size of the silver nanoparticles prepared is 8-15nm, even in shape and good in dispersity, and the silver nanoparticles has good application prospect in the fields of biology, pharmacy, catalysis and the like.

Description

The method of the synthetic Nano silver grain of a kind of grapefruit skin extract microwave

Technical field

The present invention relates to the preparation method of Nano silver grain, the method for the synthetic Nano silver grain of especially a kind of grapefruit skin extract microwave.

Background technology

In recent years, noble metal nano particles is because having unique performance such as large specific area, good interfacial effect and small-size effect, in catalysis, optics, information storage, SERS, biomarker, the aspects such as image and sensing have potential application prospect; In all metals, noble silver has best electrical conductivity and thermal conductivity, and silver nano-grain has very stable physical and chemical performance, there is very excellent performance in electricity, optics and catalysis etc. aspect numerous, many fields such as ceramic material, environment-friendly materials, coating, catalysis and SERS technology now have been widely used in, have a extensive future, therefore cause researcher's extensive concern.

Chemical method is the preparation method of at present the most frequently used Nano silver grain, use more reducing agent that sodium borohydride, hydrazine hydrate, dimethyl formamide etc. are arranged, yet these toxicity of compound are strong, seriously polluted, human body and environment are all existed to serious harm, therefore, " greenization " of nano material preparation process just seems particularly important, and replace traditional, poisonous organic compound with the green solvent of safety, environmental protection, nontoxic reducing agent and macromolecule stabilizer, just become the important research direction of Green Chemistry; Simultaneously, green synthetic noble metal nanometer material has good biocompatibility, can be more convenient, more easily in pharmacy and biomedical aspect, be applied; Nontoxic reproducible compound matter β for Raveendran etc.-D-Glucose reduction AgNO ₃solution, soluble starch, as protective agent, can obtain silver nanoparticle colloidal sol (J. Am. Chem. Soc., 2003,125,13940) after 40 ℃ of reaction 20h under the protection of atmosphere gas; The Sastry group study extract of India Cai's leaf, Neem leaf to the reduction to gold chloride, silver ion, prepared the gold, silver nano particle, and its potential application has been carried out probing into (J. Colloid Interface Sci., 2004,275,496).The edible mushroom of the use such as Phlilip, honey have synthesized gold, silver nano particle (Molecular and Biomolecidar Spectroscopy., 2009. 73,374); Up to now, there is not yet under grapefruit skin extract exists, the synthetic Nano silver grain of microwave method report.

Summary of the invention

The present invention relates to the method for the synthetic Nano silver grain of a kind of microwave, the method for the synthetic Nano silver grain of especially a kind of grapefruit skin extract microwave.

The present invention realizes by following steps:

(1) grapefruit skin extract: grapefruit skin extract is to report that with reference to Sun seminar the method for (Anal. Chem. 2012,84,5,351 5357) obtains, and it is 0.1g/L that the water dissolving is settled to concentration, in every liter of solution, contains grapefruit bark extract 0.1g;

(2) preparation AgNO ₃the aqueous solution (concentration is 1.7～8.5g/L), then measure grapefruit skin extract and the AgNO of certain volume ₃solution adds in beaker (wherein pomelo peel extract and AgNO together ₃the volume ratio of solution is 0.5～1.2:1), after mixing and stirring, be transferred in microwave reactor, under 400～700W power, react 3～30 min.

(3) reaction is cooled to room temperature after finishing, with distilled water, ethanol respectively centrifugal, wash products repeatedly after, obtain Nano silver grain.

(4) utilize X-ray diffractometer (XRD), transmission electron microscope (TEM), ultraviolet-uisible spectrophotometer (UV) to carry out micromorphology analysis to product.

Compared with prior art, the present invention has following characteristics: adopt reducing agent and the stabilizing agent of the pomelo peel extract of natural green as Nano silver grain, adopt the auxiliary synthetic method of microwave, Simple fast, and in whole preparation process, without adding any chemical reagent, preparation process has the advantages such as environmental protection, convenient and efficient, and the particle diameter of prepared Nano silver grain is 8-15nm, the granule-morphology homogeneous, favorable dispersibility; The synthetic silver nano-grain of this method has the applications well prospect in fields such as biology, pharmacy, catalysis.

The accompanying drawing explanation

The XRD diffraction spectrogram of the Nano silver grain that Fig. 1 is preparation can find out that the Nano silver grain prepared by this method is pure phase.

Fig. 2 is the TEM photo of the Nano silver grain of preparation.The size that can find out prepared Nano silver grain in photo is 8-15nm, and particle diameter is evenly distributed, granule-morphology homogeneous, favorable dispersibility.

Fig. 3, for the ultraviolet-visible spectrogram of the Nano silver grain of preparation, can observe at 450cm in spectrogram ^-1a wider absworption peak occurs, further confirmed the successful preparation of silver nano-grain.

embodiment 1

Measure the grapefruit skin extract (0.1g/L) that 30mL prepares and be poured in the 250mL beaker, then measure 30mLAgNO ₃solution (3.4g/L) adds in beaker, after continuing to be uniformly mixed liquid 20min, beaker is transferred in microwave reactor, under power 400W, reacts 30min; After having reacted, by the products therefrom centrifugation, and, after cleaning respectively 3 times with distilled water, ethanol respectively, obtain Nano silver grain.

embodiment 2

Measure the grapefruit skin extract (0.1g/L) that 36mL prepares and be poured in the 250mL beaker, then measure 30mLAgNO ₃solution (1.7g/L) adds in beaker, after continuing to be uniformly mixed liquid 20min, beaker is transferred in microwave reactor, under power 500W, reacts 20min; After having reacted, by the products therefrom centrifugation, and, after cleaning respectively 3 times with distilled water, ethanol respectively, obtain Nano silver grain.

embodiment 3

Measure the grapefruit skin extract (0.1g/L) that 40mL prepares and be poured in the 250mL beaker, then measure 50mLAgNO ₃solution (6.8g/L) adds in beaker, after continuing to be uniformly mixed liquid 20min, beaker is transferred in microwave reactor, under power 700W, reacts 3min; After having reacted, by the products therefrom centrifugation, and, after cleaning respectively 3 times with distilled water, ethanol respectively, obtain Nano silver grain.

embodiment 4

Measure the grapefruit skin extract (0.1g/L) that 20mL prepares and be poured in the 250mL beaker, then measure 40mLAgNO ₃solution (8.5g/L) adds in beaker, after continuing to be uniformly mixed liquid 20min, beaker is transferred in microwave reactor, under power 600W, reacts 12min; After having reacted, by the products therefrom centrifugation, and, after cleaning respectively 3 times with distilled water, ethanol respectively, obtain Nano silver grain.

Claims

1. the method for the synthetic silver nano-grain of a grapefruit skin extract microwave is characterized in that step is as follows:

(1) grapefruit skin extract is mixed with silver nitrate aqueous solution, stir, obtain the reaction precursor liquid solution;

(2) the reaction precursor liquid solution is transferred in microwave reactor, the heating using microwave reaction, reaction is cooled to room temperature after finishing, and centrifugation obtains Nano silver grain after cleaning.

2. a kind of grapefruit skin extract microwave as claimed in claim 1 synthesizes the method for silver nano-grain, it is characterized in that:

The concentration of described grapefruit skin extract is 0.1g/L.

3. a kind of grapefruit skin extract microwave as claimed in claim 1 synthesizes the method for silver nano-grain, it is characterized in that:

The concentration of described silver nitrate aqueous solution is 1.7～8.5g/L.

4. a kind of grapefruit skin extract microwave as claimed in claim 1 synthesizes the method for silver nano-grain, and it is characterized in that: the volume ratio of described grapefruit skin extract and silver nitrate is 0.5～1.2:1.

5. a kind of grapefruit skin extract microwave as claimed in claim 1 synthesizes the method for silver nano-grain, and it is characterized in that: the heating power of described microwave reactor is 400～700W, reaction time 3～30min that described microwave is synthetic.

6. a kind of grapefruit skin extract microwave as claimed in claim 1 synthesizes the method for silver nano-grain, it is characterized in that:

The particle diameter of described Nano silver grain is 8-15nm, granule-morphology homogeneous, favorable dispersibility.