CN112705728A - Green preparation method of silver nanorods - Google Patents
Green preparation method of silver nanorods Download PDFInfo
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- CN112705728A CN112705728A CN202110062843.4A CN202110062843A CN112705728A CN 112705728 A CN112705728 A CN 112705728A CN 202110062843 A CN202110062843 A CN 202110062843A CN 112705728 A CN112705728 A CN 112705728A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- 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 green preparation method of silver nanorods, belongs to the technical field of silver nanorod preparation, and can solve the problems of complex process, low yield and non-green environmental protection of the silver nanorods prepared by the existing seed crystal method3The addition of the solution is adjusted, and the method has important practical application value as a method for preparing the silver nano-rod in a green and large-scale manner.
Description
Technical Field
The invention belongs to the technical field of preparation of silver nanorods, and particularly relates to a method for preparing silver nanorods in a green color in a natural plant extract.
Background
In recent years, due to the rapid development of new noble metal nano materials in the preparation technology, many excellent characteristics of metal nano materials are gradually discovered. Silver is a relatively cheap raw material in a noble metal family, and naturally becomes the most research hotspot with development potential, and silver nano materials have the shapes of spheres, triangles, rods, cubes and the like, wherein silver nanorods have the optical characteristics of surface plasmon resonance, so that the silver nanorods can be applied to the aspects of optical transmission, optical imaging, biological detection and the like, and are attracted by researchers.
The preparation method of the silver nano material comprises an electrochemical method, a chemical reduction method, a sol-gel method, a coprecipitation method, a hydrothermal method, a polyol method and the like, and a certain stabilizing agent or a protecting agent is generally required to be added in the preparation process, so that the organic matters can cause environmental pollution and harm to human bodies and increase the cost. The classical method for preparing the silver nanorods is a seed crystal method reported by Murphy, the yield of the method is low, and the steps are complex, so that the development of the method for preparing the silver nanorods, which is green and environment-friendly and is simple and convenient to operate, has certain research significance.
The yellow flower is taken as an edible flower, contains abundant flavonoid compounds, has reducibility and biodegradability, is non-toxic, does not cause pollution to the environment, and is hopeful to be used as a raw material for preparing the silver nano material. The application aims to prepare the silver nanorods by using flavonoid compounds of the extract of daylily as a reducing agent and a protective agent.
Disclosure of Invention
The invention provides a preparation method of silver nanorods, and particularly provides a method for preparing silver nanorods in green color in natural plant extract, aiming at the problems of complex process, low yield and no green environmental protection in the existing seed crystal method for preparing silver nanorods.
The invention adopts the following technical scheme:
a green preparation method of silver nanorods comprises the following steps:
first, extraction of flavonoids
Grinding dry daylily into powder, weighing 5.0 g of ground daylily, placing in a 250 mL round-bottom flask, adding 125 mL of distilled water, soaking for 90 minutes, adding zeolite, repeatedly heating and refluxing for three times, two hours each time, cooling, performing suction filtration for three times by using a suction bottle, and collecting an extracting solution to obtain 1000 mL of daylily extracting solution for later use;
second, preparing silver nano-rod
Firstly, preparing a silver nitrate solution with the concentration of 0.1mol/L, transferring 50mL of daylily extract into a 100 mL volumetric flask, adding the silver nitrate solution into the volumetric flask, then carrying out volume metering by using deionized water, placing the volumetric flask in an environment with sufficient light for continuous reaction for two hours at normal temperature, carrying out centrifugal separation in a centrifugal tube after the reaction is finished, wherein the rotating speed is 12000 r/min, the time is 5 min, and finally alternately cleaning a product obtained by centrifugation by using absolute ethyl alcohol and deionized water for three times, and airing to obtain the product.
The volume of the silver nitrate solution in the second step is 0.5-5 mL.
The invention has the following beneficial effects:
the whole preparation process is convenient to operate, the process is simple, the method can be used for green batch preparation of the silver nanorods, the defects of complex process, low yield, greenness, environmental friendliness and the like of the traditional crystal seed method are overcome, and the prepared silver nanorods can pass through AgNO in length3The addition of the solution is adjusted, and the method has important practical application value as a method for preparing the silver nano-rod in a green and large-scale manner.
Drawings
Fig. 1 is a graph of the ultraviolet-absorption spectra of silver nanoparticles prepared with different silver nitrate concentrations, wherein: the labels 1-4 are ultraviolet images with silver nitrate concentrations of 0.5 mmol/L, 1.0 mmol/L, 5 mmol/L, and 10 mmol/L, respectively.
Fig. 2 is a graph of the uv-absorption spectra of silver nanoparticles prepared at different illumination times, wherein: the reference numbers 1-6 refer to ultraviolet images with illumination time of 1h, 2h, 3h, 4 h, 8 h and 12h respectively.
FIG. 3 is an SEM image of silver nanorods with silver nitrate concentration of 0.5 mmol/L and illumination time of 2 h.
FIG. 4 is an SEM image of silver nanorods with silver nitrate concentration of 1 mmol/L and illumination time of 2 h.
FIG. 5 is an SEM image of silver nanorods with a silver nitrate concentration of 5 mmol/L and an illumination time of 2 h.
FIG. 6 is an SEM image of silver nanorods with a silver nitrate concentration of 10 mmol/L and an illumination time of 2 h.
FIG. 7 is an SEM image of silver nanorods with silver nitrate concentration of 5 mmol/L at illumination time of 1h (A), 2h (B), 3h (C), 12h (D).
FIG. 8 is an SEM image of silver nanorods prepared in large batches (illumination time 2h, silver nitrate concentration 5 mmol/L).
Fig. 9 is an XRD pattern of the silver nanorods prepared by the present invention.
FIG. 10 is an EDX diagram of silver nanorods prepared according to the present invention.
Detailed Description
The extraction of the flavonoid compounds in the day lily of the invention comprises the following steps:
grinding flos Hemerocallis into powder, accurately weighing 5.0000 g of the grinded flos Hemerocallis in 250 mL round bottom flask, adding 125 mL distilled water, soaking for 90 min, and heating and refluxing for three times, two hours each time. After cooling, carrying out suction filtration for three times, and collecting the extracting solution for later use.
Accurately transferring 5mL of the suction-filtered yellow flower extract into a 25 mL volumetric flask by using a pipette, adding 1.0 mL of 5% sodium nitrite, uniformly mixing, standing for 6 min, adding 1.0 mL of 10% aluminum nitrate solution, shaking up, standing for 6 min, adding 10.0 mL of 1% sodium hydroxide solution, adding distilled water to a scale, shaking up, standing for 15 min, and measuring the absorbance at 510 nm by using an ultraviolet spectrophotometer to be 0.177. Substituting into a standard curve regression equation: y =12.29688X +0.045889(R =0.99988), and the concentration of flavonoid compounds in the obtained day lily extract is 10.7X 10-3 mg/L。
Example 1: firstly, accurately preparing 0.1 mol/LAgNO3Transferring 50mL of daylily extract into 100 mL volumetric flask, and adding into volumetric flask0.5 mL of 0.1mol/L silver nitrate solution is added, and then the volume is determined by deionized water. At normal temperature, the volumetric flask is placed in an environment with sufficient light for continuous reaction for two hours, and centrifugal separation is carried out in a centrifugal tube after the reaction is finished, wherein the rotating speed is 12000 r/min, and the time is 5 min. And finally, alternately cleaning the product obtained by centrifugation with absolute ethyl alcohol and deionized water for three times, and airing to obtain the product.
Example 2: firstly, accurately preparing 0.1 mol/LAgNO3The solution is prepared by transferring 50mL of daylily extract into a 100 mL volumetric flask, adding 1.0 mL of 0.1mol/L silver nitrate solution into the volumetric flask, and then adding deionized water to a constant volume. At normal temperature, the volumetric flask is placed in an environment with sufficient light for continuous reaction for two hours, and centrifugal separation is carried out in a centrifugal tube after the reaction is finished, wherein the rotating speed is 12000 r/min, and the time is 5 min. And finally, alternately cleaning the product obtained by centrifugation with absolute ethyl alcohol and deionized water for three times, and airing to obtain the product.
Example 3: firstly, accurately preparing 0.1 mol/LAgNO3The solution is prepared by transferring 50mL of daylily extract into a 100 mL volumetric flask, adding 5.0 mL of 0.1mol/L silver nitrate solution into the volumetric flask, and then adding deionized water to a constant volume. At normal temperature, the volumetric flask is placed in an environment with sufficient light for continuous reaction for two hours, and centrifugal separation is carried out in a centrifugal tube after the reaction is finished, wherein the rotating speed is 12000 r/min, and the time is 5 min. And finally, alternately cleaning the product obtained by centrifugation with absolute ethyl alcohol and deionized water for three times, and airing to obtain the product.
The screening process of the invention is as follows:
1. preparing silver nanorods under different silver nitrate concentrations.
（1）0.1 mol/LAgNO3Solution preparation: 1.6987 g of silver nitrate is accurately weighed into a beaker, dissolved by a small amount of distilled water, poured into a 100 mL volumetric flask for constant volume and shaken up.
(2) Taking four 100 mL volumetric flasks, numbered A, B, C, D, precisely transferring 50.00 mL of the daylily extract into the four volumetric flasks by using a pipette, respectively adding 0.50 mL (namely, example 1), 1.00 mL (namely, example 2), 5.00 mL (namely, example 3) and 10.00 mL of 0.1mol/L silver nitrate solution into the volumetric flasks, and then fixing the volume by using deionized water.
(3) And (3) at normal temperature, simultaneously placing the four volumetric flasks on the same windowsill with sufficient light to continuously react for two hours, and after the reaction for two hours, using the day lily extract as a blank control to respectively perform ultraviolet-visible absorption spectrum detection on the solutions in the four volumetric flasks. And then pouring the residual solution into a centrifuge tube for centrifugal separation, and adjusting the rotating speed to 12000 r/min for 5 min. And finally, alternately cleaning the product obtained by centrifugation with absolute ethyl alcohol and deionized water for three times, cleaning with absolute ethyl alcohol and then drying in the air. And the product is subjected to XRD and SEM detection.
Silver nano-particles are prepared by changing the concentration of silver nitrate, namely the concentration is 0.5 mmol/L, 1 mmol/L, 5 mmol/L and 10 mmol/L, and ultraviolet-visible spectrum detection is carried out after reaction for 2 h. The results are shown in FIG. 1:
as can be seen from fig. 1: with the increase of the concentration of silver nitrate, the characteristic absorption peak of the silver nanometer gradually widens, and the characteristic absorption peak does not widen after the concentration increases to a certain value. Indicating that the size of the silver nano-particles gradually becomes larger until the maximum size is reached, and the silver nano-particles do not change.
The silver nano-particles are prepared by changing the concentration of silver nitrate, namely the concentration of the silver nitrate is 0.5 mmol/L, 1 mmol/L, 5 mmol/L and 10 mmol/L, and the silver nano-particles are detected by a scanning electron microscope after reacting for 2 hours. As a result, as shown in FIGS. 3 to 6, the prepared silver nano-rods were rod-shaped, and the prepared silver nano-rods were longest in length, 2.65 um in length, and relatively uniform when the silver nitrate concentration was 5 mmol/L. The length of the nano silver is increased and then reduced along with the concentration of the silver nitrate. In the figure, the silver nanorods have impurity ions.
2. Preparing the silver nano-rod under different illumination time.
(1) Taking six 100 mL volumetric flasks numbered 1, 2, 3, 4, 5 and 6, precisely transferring 50.00 mL of daylily extract into the six volumetric flasks by using a pipette, adding 5.00 mL of 0.1mol/L silver nitrate solution into the volumetric flasks respectively, and then fixing the volume by using deionized water.
(2) At normal temperature, the six volumetric flasks are simultaneously placed on the same windowsill with sufficient light to enable the continuous reaction time to be 1h, 2h (namely embodiment 3), 3h, 4 h, 8 h and 12h, after the reaction is finished, the day lily extract is used as a blank control, and the solutions in the four volumetric flasks are respectively subjected to ultraviolet-visible absorption spectrum detection. And then pouring the residual solution into a centrifuge tube for centrifugal separation, and adjusting the rotating speed to 12000 r/min for 5 min. And finally, alternately cleaning the product obtained by centrifugation with absolute ethyl alcohol and deionized water for three times, cleaning with absolute ethyl alcohol and then drying in the air. And the product is subjected to XRD and SEM detection.
The silver nano is prepared by changing the illumination time, namely the time is 1h, 2h, 3h, 4 h, 8 h and 12h, the concentration of silver nitrate is controlled to be 5 mmol/L, and ultraviolet-visible spectrum detection is carried out after the reaction is completed. The results are shown in FIG. 2:
as can be seen from fig. 2: the position of the maximum characteristic absorption peak of the silver nano material is gradually increased along with the prolonging of the illumination time. From 468 nm for 1h to 477 nm for 2h, 494 nm for 3h, 516 nm for 4 h, 566 nm for 8 h, 565 nm for 12 h.
The silver nano is prepared by changing the illumination time, namely the time is 1h, 2h, 3h, 4 h, 8 h and 12h, so that the concentration of silver nitrate is 5 mmol/L, and electron microscope detection is carried out after the reaction is completed. The results are shown in FIG. 7, which shows that: when the illumination time is 2h, the particles are relatively uniform and are distributed in a rod shape. When the illumination time is prolonged, the silver nanoparticles are easy to agglomerate, and the effect is poor. The crystallization degree of the silver nano is related to the flavonoid compound, and the longer the illumination time is, the worse the crystallization degree is.
The results of mass verification preparation experiments show that when the concentration of silver nitrate is controlled to be 5 mmol/L and the illumination time is 2 hours, the length-diameter ratio of the product is about 2.86 silver nanorods, the product size is uniform, and the yield is high.
XRD result analysis is performed on the prepared silver nanorods, and the result is shown in FIG. 9, and the unit cell parameters of the nano units can be obtained from FIG. 9 for analyzing the structure of the crystal. The crystal plane indices are (111), (200), (220) and (311) crystal planes in this order. The reason why the prepared silver is pure silver, the product configuration is a face-centered cubic structure and the peaks are not sharp and numerous in impurity peaks is that the flavonoid compound can influence the crystallization degree of the silver nano-particles.
The prepared silver nanorod is subjected to energy spectrum analysis, and the result is shown in fig. 10, spectral peaks of elements of carbon, nitrogen, oxygen and silver appear in a spectrogram, and the elements of carbon, nitrogen and oxygen are base elements, which indicates that the silver nanomaterial is successfully prepared, and other miscellaneous peaks except the four peaks do not appear, so that the prepared product is determined to be pure silver and has no other impurities.
The invention adopts a green preparation method, takes flavonoid compounds in the day lily extract as a reducing agent and a protective agent, and successfully synthesizes the silver nanorods. The influence of silver nitrate concentration and illumination conditions on the product morphology is investigated in the experiment, and the product is characterized by ultraviolet-visible absorption spectrum (UV-Vis), X-ray powder diffraction (XRD) and electron microscope (SEM). The study concluded the following:
(1) the UV-Vis results show a characteristic absorption peak of silver at 420-480 nm. The SEM results show that: in AgNO3The nano particles prepared when the concentration is 5 mmol/L and the illumination time is 2 hours are relatively uniform. Increasing the illumination time is not favorable for the formation of silver nanorods.
(2) The verification test shows that: the method can be applied to the mass preparation of the silver nanorods, and has high yield and uniform size.
(3) The XRD shows that the prepared product is silver with a face-centered cubic structure, but the flavonoid compound has certain influence on the crystallinity of the product. The EDX results further indicated that the product was pure silver.
Claims (2)
1. A green preparation method of silver nanorods is characterized in that: the method comprises the following steps:
first, extraction of flavonoids
Grinding dry daylily into powder, weighing 5.0 g of ground daylily, placing in a 250 mL round-bottom flask, adding 125 mL of distilled water, soaking for 90 minutes, adding zeolite, repeatedly heating and refluxing for three times, two hours each time, cooling, performing suction filtration for three times by using a suction bottle, and collecting an extracting solution to obtain 1000 mL of daylily extracting solution for later use;
second, preparing silver nano-rod
Firstly, preparing a silver nitrate solution with the concentration of 0.1mol/L, transferring 50mL of daylily extract into a 100 mL volumetric flask, adding the silver nitrate solution into the volumetric flask, then carrying out volume metering by using deionized water, placing the volumetric flask in an environment with sufficient light for continuous reaction for two hours at normal temperature, carrying out centrifugal separation in a centrifugal tube after the reaction is finished, wherein the rotating speed is 12000 r/min, the time is 5 min, and finally alternately cleaning a product obtained by centrifugation by using absolute ethyl alcohol and deionized water for three times, and airing to obtain the product.
2. The green preparation method of silver nanorods according to claim 1, characterized in that: the volume of the silver nitrate solution in the second step is 0.5-5 mL.
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