CN107840957B - Dandelion-shaped gold nanoparticle @ polyaniline nanocomposite prepared by one-pot method and preparation method and application thereof - Google Patents
Dandelion-shaped gold nanoparticle @ polyaniline nanocomposite prepared by one-pot method and preparation method and application thereof Download PDFInfo
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- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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Abstract
The invention discloses a dandelion-shaped gold nanoparticle @ polyaniline nanocomposite material prepared by a one-pot method and a preparation method and application thereof. The method comprises the following steps: (a) uniformly dispersing aniline monomer in inorganic acid to obtain aniline monomer dispersion liquid; (b) adding chloroauric acid solution as gold source into aniline monomer dispersion liquid under the condition of continuous stirring; (c) continuously stirring for reaction until a light blue product is obtained, centrifuging, washing and drying to obtain the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite. The conductive noble metal nano particles @ high-molecular polymer with uniform appearance and stable structure and performance is prepared by adopting a one-pot method, the method is simple and easy to implement, low in cost, mild in condition and suitable for large-scale production, and the obtained composite material is used as an electrode modification material, has good conductivity and electrochemical activity, can be applied to catalytic detection of heavy metal pollutants on copper, and has the advantages of high sensitivity, reusability and the like.
Description
Technical Field
The invention relates to the field of preparation of conductive polymer/metal nanoparticle composite materials, in particular to a dandelion-shaped gold nanoparticle @ polyaniline nanocomposite material prepared by a one-pot method and a preparation method and application thereof.
Background
Polyaniline (Polyaniline) has a p-electron conjugated structure, belongs to one of conductive polymer materials, has special electrical and optical properties, and can have conductivity and electrochemical properties after being doped. Polyaniline is widely researched and applied due to the structural characteristics of easy availability of raw materials, simple synthesis process, good chemical and environmental stability and the like.
The noble metal nano-particles have unique optical and electrical properties, so that the noble metal nano-particles can be widely applied to the fields of catalysis, medicine, biology and sensing. In recent years, high-performance photoelectric, sensing and storage devices can be prepared by compounding noble metal nanoparticles with conductive polymers such as polypyrrole (PPy), Polyaniline (PANI), polythiophene and the like. Therefore, the research on the noble metal nano-particles @ conductive polymer composite material has received extensive attention. Among them, gold nanoparticles are the focus of research in the field of electrode materials and biosensors due to their advantages of non-toxicity, good biocompatibility, excellent conductivity, etc. In addition, the morphology of the noble metal nanoparticles affects the properties to some extent, and the size of the nanoparticles and the distribution uniformity thereof in the conductive polymer are the main factors determining the performance of the composite material. The size and uniformity of the nano particles are effectively controlled, the agglomeration is reduced, the morphological characteristics of the compound are regulated and controlled, and the stability and catalytic activity of the noble metal nano particles can be enhanced. Therefore, it is necessary to control the size of the noble metal nanoparticles and the morphological characteristics of the complex for practical application.
At present, the preparation method of the noble metal nanoparticle @ conductive polymer composite material mainly comprises the following steps: in-situ polymerization, electrochemical deposition, blending, self-assembly techniques, chemical reduction, and the like. The chinese patent publication No. CN104119527A discloses a gold-polyaniline nanocomposite particle and a preparation method thereof, the structure of the composite is that the surface of a gold nanoparticle is wrapped with a polyaniline layer, the preparation method requires a low temperature condition of ice bath, and the time consumption is long through a complex separation process, and the size of the obtained golf spherical composite nanoparticle is 10-20 nm. Chinese patent publication No. CN105461920A discloses a method for synthesizing echinoid gold nanoparticles and spherical polyaniline by one-pot method and application thereof, the preparation method needs additional addition of stabilizer and oxidant, the operation is complicated, and echinoid gold nanoparticles and spherical polyaniline can be obtained respectively with different separation processes. The method has the defects of complex operation and incapability of meeting large-scale industrial production. Therefore, the discussion of the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite material and the application thereof which are convenient and easy to realize has very important significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a dandelion-shaped gold nanoparticle @ polyaniline nanocomposite prepared by a one-pot method and a preparation method and application thereof.
The purpose of the invention is realized by the following technical scheme.
The method for preparing the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite by the one-pot method comprises the following steps:
(a) uniformly dispersing aniline monomer in inorganic acid to obtain aniline monomer dispersion liquid;
(b) adding chloroauric acid solution as gold source into aniline monomer dispersion liquid under the condition of continuous stirring;
(c) continuously stirring for reaction until a light blue product is obtained, then centrifugally separating and collecting a reaction product, and then washing and drying to obtain the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite.
Preferably, in the step (a), the inorganic acid is one or two of hydrochloric acid and nitric acid, and the concentration of the inorganic acid is 0.5-1.0 mol/L.
Preferably, in the step (b), the concentration of the chloroauric acid solution is 6-12 mmol/L.
Preferably, in the steps (a) and (b), the volume ratio of the aniline monomer to the inorganic acid to the chloroauric acid solution is 1: (50-100): (10-20).
Preferably, in the step (c), the stirring reaction time is 6-12 h.
Preferably, in the step (c), the centrifugation is performed at 8000-10000 rpm for 10-15 min.
Preferably, in step (c), the washing is sequentially with absolute ethanol, water and N-methylpyrrolidone.
Preferably, in the step (c), the drying is vacuum drying at 60-80 ℃ for 8-12 h.
The dandelion-shaped gold nanoparticle @ polyaniline nanocomposite prepared by the method is applied to electrochemical analysis and detection of trace heavy metal ions.
Compared with the prior art, the invention has the following technical effects:
1. according to the invention, aniline monomer polymerization and chloroauric acid action are directly adopted, no reducing agent is added, and in-situ reduction is directly carried out, so that the obtained gold nanoparticles are uniformly dispersed and uniform in size, the thickness of the gold nanoparticle @ polyaniline composite film is controllable, the technical problem of gold nanoparticle agglomeration can be solved, and the application range of the noble metal particle @ conductive polymer is enriched.
2. The invention has the advantages of low cost, simple operation, mild condition, stable structure and performance of the obtained composite material, and suitability for large-scale production.
3. The dandelion-shaped gold nanoparticle @ polyaniline nanocomposite material obtained by the invention can be specifically used for rapid trace analysis and detection of heavy metal ion copper.
Drawings
Fig. 1 is an XRD pattern of the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite obtained in example 1 of the present invention.
Fig. 2 is an SEM image of the taraxacum-shaped gold nanoparticles @ polyaniline nanocomposite obtained in example 1 of the present invention.
Fig. 3a is a TEM image of the taraxacum-shaped gold nanoparticle @ polyaniline nanocomposite obtained in example 1 of the present invention.
Fig. 3b is a high magnification TEM image of the dandelion-like gold nanoparticle @ polyaniline nanocomposite obtained in example 1 of the present invention.
Fig. 4 is a high-resolution TEM image of the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite obtained in example 1 of the present invention.
FIG. 5 is a graph showing the peak profile obtained by square wave anodic stripping voltammetry in example 2 of the present invention.
Detailed Description
The embodiments of the present invention will be further described with reference to the following examples and drawings, but the embodiments of the present invention are not limited thereto.
Example 1
The method for preparing the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite by the one-pot method specifically comprises the following steps:
uniformly dispersing 0.18mL of aniline monomer in 18mL of 0.5mol/L hydrochloric acid solution under the condition of normal temperature, dropwise adding 1.8mL of 6mmol/L chloroauric acid solution under the condition of continuous stirring, reacting for 12h to obtain a blue product, centrifuging the product at the rotation speed of 8000 rpm for 15min, sequentially and respectively washing with absolute ethyl alcohol, deionized water and N-methylpyrrolidone until filtrate is colorless, and drying in vacuum at 60 ℃ for 12h to obtain the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite.
And (3) testing the structural performance: the gold nanoparticle @ polyaniline nanocomposite material is characterized by an XRD (solid powder X-ray diffraction analysis) technology (see figure 1), a wider peak between 10-30 degrees at a 2 theta position appears in the material, and the wider peak is a characteristic peak of polyaniline, and in addition, the characteristic diffraction peaks of the composite material are 2 theta =38.2 degrees of Au (111), 2 theta =44.3 degrees of Au (200), and 2 theta =64.8 degrees of Au (220). XRD results show that the compound consists of gold nanoparticles and polyaniline. The material was characterized using Scanning Electron Microscopy (SEM) techniques (see fig. 2), and was shown to be a structure composed of rods and spheres. The rod size of the composite material is 0.9-1.17 μm, and the spherical size is 300-500 nm. The material is characterized by adopting a Transmission Electron Microscope (TEM) technology (see fig. 3a and fig. 3 b), and the result shows that the gold nanoparticle @ polyaniline compound is similar to a dandelion shape, the size of the gold nanoparticle is between 5 and 20nm, the gold nanoparticle is uniformly distributed in the polyaniline, and the TEM result is the same as the SEM result. In addition, the lattice fringes showed Au (111) crystal plane characteristics of d =0.235nm and Au (220) crystal plane characteristics of d =0.144nm (see fig. 4), indicating that the gold nanoparticles are uniformly wrapped in the polyaniline film.
Testing heavy metal detection performance: the obtained dandelion-shaped gold nanoparticle @ polyaniline nanocomposite is used for analyzing and detecting heavy metal copper in tap water. The specific experimental steps are as follows:
accurately weighing 4 mg of the gold nanoparticle @ polyaniline nanocomposite prepared by the embodiment by using an analytical balance, adding 2mL of 0.125wt% Nafion ethanol solution, ultrasonically vibrating to uniformly disperse the material, then using a pipettor to take 5 muL of the material to be smeared on the surface of the polished glassy carbon electrode, and baking by using an infrared lamp for later use. Heavy metal detection adopts Square Wave Anodic Stripping Voltammetry (SWASV), a three-electrode system is formed by a glassy carbon electrode, a counter electrode (platinum electrode) and an Ag-AgCl electrode, 10mL of acetic acid-sodium acetate buffer solution (pH 4.5) is added into an electrolytic cell with a stirrer, three electrodes are immersed in the buffer solution, and square wave anodic stripping voltammetry detection parameters of an electrochemical analyzer are set: amplitude: 25 mV; potential increment: 4 mV; frequency: 15 mV; the enrichment potential is-1.2V; the enrichment time is 360s, and the stirring speed is 500 r/min; standing for 15 s; the initial potential for dissolution was-1.0V, and the final potential was 0V. And sequentially measuring current response values of 0, 1, 5, 1.0, 15, 20, 30 and 40 mug/L to obtain a working curve (see figure 5). And then modifying the electrode again, taking 5 mL of tap water, mixing 5 mL of acetic acid-sodium acetate buffer solution with pH of 4.5, determining the mode in the same process as the working curve, and then sequentially adding three times of standard samples to obtain the copper content in the tap water of 0.53 mug/L. Meets the national drinking water standard.
Example 2
The preparation method for preparing the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite by the one-pot method specifically comprises the following steps:
uniformly dispersing 0.18mL of aniline monomer in 9mL of 1.0 mol/L hydrochloric acid solution at normal temperature, dropwise adding 3.6mL of 12mmol/L chloroauric acid solution under the condition of continuous stirring, reacting for 6h to obtain a blue product, centrifuging the product at the rotation speed of 10000rpm for 10min, sequentially and respectively washing with absolute ethyl alcohol, water and N-methylpyrrolidone until filtrate is colorless, and drying in vacuum at 80 ℃ for 8h to obtain the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite.
And (3) testing the structural performance: the gold nanoparticle @ polyaniline nanocomposite obtained in this example was characterized by an XRD (solid powder X-ray diffraction analysis) technique, and the XRD result is similar to that of fig. 1, indicating that the composite consisted of gold nanoparticles and polyaniline. The material was characterized using Scanning Electron Microscopy (SEM) techniques and, as a result, was similar to figure 2, showing a structure composed of rods and spheres. The material was characterized by Transmission Electron Microscopy (TEM) and the results were similar to those in fig. 3a and 3b, showing that the gold nanoparticles @ polyaniline complex was similar to dandelion and evenly distributed in polyaniline.
Testing heavy metal detection performance: the obtained dandelion-shaped gold nanoparticle @ polyaniline nanocomposite is used for analyzing and detecting heavy metals of lead and cadmium in lake water. The specific experimental steps are as follows:
accurately weighing 4 mg of the gold nanoparticle @ polyaniline nanocomposite prepared by the embodiment by using an analytical balance, adding 2mL of 0.125wt% Nafion ethanol solution, ultrasonically vibrating to uniformly disperse the material, then taking 5 muL by using a pipettor to smear on the surface of the polished glassy carbon electrode, and baking by using an infrared lamp for later use. Heavy metal detection adopts a Square Wave Anodic Stripping Voltammetry (SWASV), a glassy carbon electrode, a counter electrode (platinum electrode) and Ag-AgCl to form a three-electrode system, 10mL of acetic acid-sodium acetate buffer solution (pH4.5) is added into an electrolytic cell with a stirrer, three electrodes are immersed in the buffer solution, and square wave anodic stripping voltammetry detection parameters of an electrochemical analyzer are set as follows: amplitude: 25 mV; potential increment: 4 mV, frequency: 15 mV; the enrichment potential is-1.2V; the enrichment time is 360s, and the stirring speed is 500 r/min; standing for 15 s; the initial potential for dissolution was-1.0V, and the final potential was 0V. And sequentially measuring current response values of 0, 1, 5, 1.0, 15, 20, 30 and 40 mug/L to obtain a working curve. And then modifying the electrode again, taking 8mL of lake water, mixing 2mL of acetic acid-sodium acetate buffer solution with pH of 4.5, determining the mode in the same process as the working curve, and then sequentially adding three standard samples to obtain lake water with copper content of 2.8 mug/L respectively.
The other implementation steps are the same as in example 1.
Example 3
The preparation method for preparing the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite by the one-pot method specifically comprises the following steps:
uniformly dispersing 0.18mL of aniline monomer in 12mL of 0.75 mol/L hydrochloric acid solution at normal temperature, dropwise adding 2.7mL of 9mmol/L chloroauric acid solution under the condition of continuous stirring, reacting for 9h to obtain a blue product, centrifuging the product at the rotating speed of 9000 rpm for 12.5min, sequentially and respectively washing with absolute ethyl alcohol, water and N-methylpyrrolidone until the filtrate is colorless, and drying in vacuum at 70 ℃ for 10h to obtain the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite.
And (3) testing the structural performance: the gold nanoparticle @ polyaniline nanocomposite obtained in this example was characterized by an XRD (solid powder X-ray diffraction analysis) technique, and the XRD result is similar to that of fig. 1, indicating that the composite consisted of gold nanoparticles and polyaniline. The material was characterized using Scanning Electron Microscopy (SEM) techniques and, as a result, was similar to figure 2, showing a structure composed of rods and spheres. The material was characterized by Transmission Electron Microscopy (TEM) and the results were similar to those in fig. 3a and 3b, showing that the gold nanoparticles @ polyaniline complex was similar to dandelion and evenly distributed in polyaniline.
Testing heavy metal detection performance: the obtained dandelion-shaped gold nanoparticle @ polyaniline nanocomposite is used for analyzing and detecting heavy metals of lead and cadmium in lake water. The specific experimental steps are as follows:
accurately weighing 4 mg of the gold nanoparticle @ polyaniline nanocomposite material obtained in the embodiment by using an analytical balance, adding 2mL of 0.125wt% Nafion ethanol solution, ultrasonically vibrating to uniformly disperse the material, then taking 5 muL by using a pipettor to smear the material on the surface of the polished glassy carbon electrode, and baking by using an infrared lamp for later use. Heavy metal detection adopts a Square Wave Anodic Stripping Voltammetry (SWASV), a glassy carbon electrode, a counter electrode (platinum electrode) and Ag-AgCl to form a three-electrode system, 10mL of acetic acid-sodium acetate buffer solution (pH4.5) is added into an electrolytic cell with a stirrer, three electrodes are immersed in the buffer solution, and square wave anodic stripping voltammetry detection parameters of an electrochemical analyzer are set as follows: amplitude: 25 mV; potential increment: 4 mV, frequency: 15 mV; the enrichment potential is-1.2V; the enrichment time is 360s, and the stirring speed is 500 r/min; standing for 15 s; the initial potential for dissolution was-1.0V, and the final potential was 0V. And sequentially measuring current response values of 0, 1, 5, 1.0, 15, 20, 30 and 40 mug/L to obtain a working curve. And then modifying the electrode again, taking 9mL of electroplating wastewater, mixing 1 mL of acetic acid-sodium acetate buffer solution with pH of 4.5, determining the mode in the same process as the working curve, and then sequentially adding three standard samples to obtain lake water with copper content of 10.4 mug/L respectively.
The other implementation steps are the same as in example 1.
Claims (9)
1. The method for preparing the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite by the one-pot method is characterized by comprising the following steps of:
(a) uniformly dispersing aniline monomer in inorganic acid to obtain aniline monomer dispersion liquid;
(b) adding chloroauric acid solution as gold source into aniline monomer dispersion liquid under the condition of continuous stirring;
(c) continuously stirring for reaction until a light blue product is obtained, then centrifugally separating and collecting a reaction product, and then washing and drying to obtain the dandelion-shaped gold nanoparticle @ polyaniline nanocomposite;
in the step (a), the concentration of the inorganic acid is 0.5-1.0 mol/L;
in the step (b), the concentration of the chloroauric acid solution is 6-12 mmol/L.
2. The method according to claim 1, wherein in step (a), the inorganic acid is one or both of hydrochloric acid and nitric acid.
3. The method according to claim 1, wherein the volume ratio of the aniline monomer, the inorganic acid and the chloroauric acid solution in the steps (a) and (b) is 1: (50-100): (10-20).
4. The method according to claim 1, wherein in the step (c), the stirring reaction time is 6-12 h.
5. The method according to claim 1, wherein in the step (c), the centrifugation is performed at 8000-10000 rpm for 10-15 min.
6. The method according to claim 1, wherein in step (c), the washing is sequentially with absolute ethanol, water and N-methylpyrrolidone.
7. The method according to claim 1, wherein in the step (c), the drying is performed at 60-80 ℃ for 8-12 h under vacuum.
8. A taraxacum-like gold nanoparticle @ polyaniline nanocomposite prepared by the method of any one of claims 1-7.
9. The dandelion-shaped gold nanoparticle @ polyaniline nanocomposite material as claimed in claim 8, which is applied to electrochemical analysis and detection of trace heavy metal ions.
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