CN113004541A - Method for preparing graphene oxide-polyaniline-gold nanoparticle solution - Google Patents
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Abstract
The method for preparing the graphene oxide-polyaniline-gold nanoparticle nanocomposite solution comprises the following steps: s11, preparing graphene oxide powder; s12, preparing a graphene oxide-polyaniline polymer; s13, preparing a gold nanoparticle solution; s14, preparing graphene oxide-polyaniline-gold nanoparticle nano composite powder; s15, dispersing the graphene oxide-polyaniline-gold nanoparticle nanocomposite powder into a chitosan solution to form the graphene oxide-polyaniline-gold nanoparticle nanocomposite solution. According to the method for preparing the graphene oxide-polyaniline-gold nanoparticle nanocomposite solution, provided by the disclosure, the graphene oxide has a large specific surface area, the gold nanoparticles have good conductivity, the polyaniline has good conductivity, and a 3D (three-dimensional) network structure can be provided, so that the specific surface area of the composite is increased, and the graphene oxide-polyaniline-gold nanoparticle nanocomposite is prepared by a hydrothermal method through the synergistic effect of the graphene oxide, the gold nanoparticles and the polyaniline.
Description
Technical Field
The present disclosure relates to a method of preparing graphene oxide-polyaniline-gold nanoparticle nanocomposite solutions.
Background
Nitrite (NO)2 -) Is a highly toxic inorganic pollutant and can cause various human diseases. Nitrites are widely distributed in industrial, agricultural, environmental, food and even physiological systems. Nitrite, which has been used as a preservative in meat based food products, has been considered as a carcinogen. Nitrite poisoning is rapidly developed, the incubation period is generally 1-3 hours, and the main characteristic of the poisoning is cyanosis caused by hypoxia, such as lips, tongue tips and fingertips, and severe cases of conjunctiva, face and whole skin are cyanosis. Dizziness, headache, asthenia, accelerated sleepiness or dysphoria due to heartbeat, dyspnea, nausea, vomiting, abdominal pain, diarrhea, coma, convulsion, and incontinence of stool and urine in severe cases, and can die due to respiratory exhaustion. Therefore, analytical detection methods for nitrite are also of great interest.
At present, the determination for detecting nitrite at home and abroad mainly comprises a national standard titration method, a spectrophotometry method, a fluorescence spectrometry method, a chemiluminescence method, an electrochemical method and the like. However, these methods have more or less disadvantages. Therefore, the development of a simple, sensitive, highly selective, economical method for detecting nitrite, which is suitable for environmental monitoring, food industry and clinical diagnosis, is urgently needed. Therefore, establishing an accurate and effective nitrite detection method has important application value and practical significance, and the premise to establish the accurate and effective nitrite detection method is how to prepare the graphene oxide-polyaniline-gold nanoparticle solution.
Disclosure of Invention
The purpose of the present disclosure is to overcome the disadvantages of the prior art and provide a method for preparing a graphene oxide-polyaniline-gold nanoparticle nanocomposite solution.
The method for preparing the graphene oxide-polyaniline-gold nanoparticle nano composite solution comprises the following steps:
s11, preparing graphene oxide powder;
s12, preparing a graphene oxide-polyaniline nano-composite;
s13, preparing a gold nanoparticle solution;
s14, preparing graphene oxide-polyaniline-gold nanoparticle nano composite powder;
s15, dispersing the graphene oxide-polyaniline-gold nanoparticle nanocomposite powder into a chitosan solution to form the graphene oxide-polyaniline-gold nanoparticle nanocomposite solution.
Wherein, in step S11, the method of preparing graphene oxide powder includes:
graphite powder is used as a raw material, and an ultrasonic stripping dispersion method is adopted to synthesize graphene oxide in an ultrasonic bath.
Wherein, in step S13, the method for preparing gold nanoparticle solution comprises:
taking 0.5-1mL HAuCl with the mass fraction of 1%4Diluting the solution to 95-100mL by ultrapure water, heating to boil, stirring, adding 3-7mL trisodium citrate solution, keeping boiling, stirring for 10-20min, removing heat source, continuing stirring, slowly cooling to room temperature to obtain gold nanoparticle solution, and storing in a container at 2-6 ℃.
Wherein, in step S12, the method for preparing the graphene oxide-polyaniline nanocomposite comprises:
taking 3-7mg of the graphene oxide powder prepared in the step S11, and ultrasonically dispersing and dissolving the graphene oxide powder by 8-12mL of deionized water to form a solution with the concentration of 0.3-0.7mg mL-1The solution of (1);
to the concentration of 0.3-0.7mg mL-1Adding aniline into the solution, stirring in ice bath for 25-35min, and adding 1.0mol L of ammonium persulfate containing 0.018g-1Stirring the solution for 20 to 28 hours at room temperature with 2.4mL of HCl to form a graphene oxide-polyaniline nano-composite solution;
and centrifuging and washing the graphene oxide-polyaniline nano composite solution, and drying for 3h at 60 ℃ in a vacuum tube oven to form the graphene oxide-polyaniline polymer.
Wherein, in step S14, the preparing graphene oxide-polyaniline-gold nanoparticle nanocomposite powder comprises:
and (3) taking 2-8mL of the gold nanoparticle solution prepared in the step S13, adding 2-8mg of the graphene oxide-polyaniline nanocomposite prepared in the step S12, stirring for 9-15h, centrifuging and washing the product, and drying in a vacuum tube oven at 50-70 ℃ for 2-4h to obtain graphene oxide-polyaniline-gold nanoparticle nanocomposite powder.
Wherein, in step S15, the dispersing the graphene oxide-polyaniline-gold nanoparticle nanocomposite powder in a chitosan solution includes:
dissolving the graphene oxide-polyaniline-gold nanoparticle nano-composite powder into a chitosan solution with the mass fraction of 0.2-0.7% to form a graphene oxide-polyaniline-gold nanoparticle nano-composite solution with the concentration of 8-10 mg/mL.
The implementation of the present disclosure includes the following technical effects:
according to the method for preparing the graphene oxide-polyaniline-gold nanoparticle nanocomposite solution, provided by the disclosure, the graphene oxide has a large specific surface area, the gold nanoparticles have good conductivity, and the polyaniline has good conductivity, and the graphene oxide-polyaniline-gold nanoparticle nanocomposite is prepared by a hydrothermal method through the synergistic effect of the graphene oxide, the gold nanoparticles and the polyaniline.
Drawings
FIG. 1 is a graph of a fitted standard of an embodiment of the present disclosure.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The implementations described in the exemplary embodiments below are not intended to represent all implementations consistent with the present disclosure. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the present disclosure, as detailed in the appended claims.
The method for preparing the graphene oxide-polyaniline-gold nanoparticle nano composite solution comprises the following steps:
s11, preparing graphene oxide powder;
s12, preparing a graphene oxide-polyaniline nano-composite;
s13, preparing a gold nanoparticle solution;
s14, preparing graphene oxide-polyaniline-gold nanoparticle nano composite powder;
s15, dispersing the graphene oxide-polyaniline-gold nanoparticle nano composite powder into a chitosan solution to form the graphene oxide-polyaniline-gold nanoparticle solution.
According to the method for preparing the graphene oxide-polyaniline-gold nanoparticle nanocomposite solution, provided by the disclosure, the graphene oxide has a large specific surface area, the gold nanoparticles have good conductivity, and the polyaniline has good conductivity, and the graphene oxide-polyaniline-gold nanoparticle nanocomposite is prepared by a hydrothermal method through the synergistic effect of the graphene oxide, the gold nanoparticles and the polyaniline.
In one embodiment, in step S11, the method of preparing graphene oxide powder includes:
graphite powder is used as a raw material, and an ultrasonic stripping dispersion method is adopted to synthesize graphene oxide in an ultrasonic bath.
In one embodiment, in step S13, the method of preparing a gold nanoparticle solution includes:
taking 0.5-1mL HAuCl with the mass fraction of 1%4For solutionsDiluting with ultrapure water to 95-100mL, heating to boiling, stirring, adding 3-7mL trisodium citrate solution, keeping boiling, stirring for 10-20min, removing heat source, stirring, slowly cooling to room temperature to obtain gold nanoparticle solution, and storing in a container at 2-6 deg.C.
In one embodiment, in step S12, the method of preparing a graphene oxide-polyaniline nanocomposite includes:
taking 3-7mg of the graphene oxide powder prepared in the step S11, and ultrasonically dispersing and dissolving the graphene oxide powder by 8-12mL of deionized water to form a solution with the concentration of 0.3-0.7mg mL-1The solution of (1);
to the concentration of 0.3-0.7mg mL-1Adding aniline into the solution, performing ice bath, stirring for 25-35min, and adding 2.4mL of 1.0mol L-1HCl is stirred for 20-28 hours at room temperature to form graphene oxide-polyaniline nano-composite solution;
and centrifuging and washing the graphene oxide-polyaniline nano-composite solution, and drying for 3h at 60 ℃ in a vacuum tube oven to form the graphene oxide-polyaniline nano-composite.
In one embodiment, in step S14, the preparing graphene oxide-polyaniline-gold nanoparticle nanocomposite powder includes:
and (3) taking 2-8mL of the gold nanoparticle solution prepared in the step S13, adding 2-8mg of the graphene oxide-polyaniline nanocomposite prepared in the step S12, stirring for 9-15h, centrifuging and washing the product, and drying in a vacuum tube oven at 50-70 ℃ for 2-4h to obtain graphene oxide-polyaniline-gold nanoparticle nanocomposite powder.
In one embodiment, in step S15, the dispersing the graphene oxide-polyaniline-gold nanoparticle nanocomposite powder in a chitosan solution includes:
dissolving the graphene oxide-polyaniline-gold nanoparticle nano composite powder into a chitosan solution with the mass fraction of 0.2-0.7% to form a graphene oxide-polyaniline-gold nanoparticle nano composite solution with the concentration of 0.4-1.4 mg/mL.
The method for detecting nitrite by electrochemical method of the present disclosure will be specifically described in the following specific examples.
1. Preparing a solution of the graphene oxide-polyaniline-gold nanoparticle nano-composite.
Firstly, graphite powder is taken as a raw material, and an ultrasonic stripping dispersion method is adopted to synthesize graphite oxide in an ultrasonic bath; then taking 5mg of graphene oxide powder, and ultrasonically dispersing and dissolving the graphene oxide powder by 10mL of deionized water to form a solution with the concentration of 0.5mg mL-1Adding aniline into the solution, carrying out ice bath, stirring for 30min, then carrying out nano-composite stirring for 24h at room temperature to form a graphene oxide-polyaniline nano-composite solution, centrifuging and washing the graphene oxide-polyaniline nano-composite solution, drying the graphene oxide-polyaniline nano-composite solution for 3h at 60 ℃ in a vacuum tube oven to form a graphene oxide-polyaniline nano-composite, then taking 5mg of the graphene oxide powder, and carrying out ultrasonic dispersion and dissolution by using 10mL of deionized water to form the graphene oxide-polyaniline nano-composite with the concentration of 0.5mg mL-1The solution of (1); then 1mL of HAuCl with the mass fraction of 1 percent is taken4Diluting the solution to 100mL by using ultrapure water, heating to boil, stirring, adding 5mL of trisodium citrate solution, keeping boiling, stirring for 15min, removing a heat source, continuously stirring, slowly cooling to room temperature to obtain a gold nanoparticle solution, and storing in a container at 4 ℃; then taking 5mL of the obtained gold nanoparticle solution, adding 5mg of the graphene oxide-polyaniline polymer, stirring for 12 hours, centrifuging and washing the product, and drying for 3 hours at 60 ℃ in a vacuum tube oven to obtain graphene oxide-polyaniline-gold nanoparticle powder; and then dissolving the graphene oxide-polyaniline-gold nanoparticle powder into a chitosan solution with the mass fraction of 0.5% to form a graphene oxide-polyaniline-gold nanoparticle nano-composite solution with the concentration of-1.0 mg/mL.
2. Preparing a nitrite sensor:
firstly, polishing a glassy carbon electrode into a mirror surface; then the polished glassy carbon electrode is sequentially treated with diluted HNO with the concentration of 0.5mol/L3Carrying out ultrasonic cleaning on absolute ethyl alcohol and distilled water, and naturally airing; finally, 5.0 mu L of the graphene oxide-polyaniline-gold nanoparticle nano-particles are dripped into the dried glassy carbon electrodeAnd naturally airing the compound solution at room temperature to obtain the nitrite sensor.
3. Fitting a standard curve:
an Ag/AgCl electrode is used as a reference electrode, a Pt electrode is used as a counter electrode, a nitrite sensor is used as a working electrode, a phosphate buffer solution with the concentration of 0.1mol/L, pH of 6 is used as a supporting electrolyte for electrochemical detection, peak current values with different concentrations are detected, the concentration of a nitrite standard solution is used as an abscissa, the peak current values are used as an ordinate, and a fitting standard curve is shown in figure 1.
4. And detecting the nitrite in the solution to be detected according to the standard curve.
The reliability verification of the electrochemical detection of nitrite provided by the present disclosure:
1. and (3) verifying linear correlation:
the standard curve obtained in the specific example of the present disclosure as shown in fig. 1 was plotted by origin 8.0 software, and the formula of the fitted standard curve was: y is 0.65+113.14X, linear correlation coefficient R20.9711, and Y25.51 +21.85X, linear correlation coefficient R20.9953, where X is the concentration (mol/L) of nitrite and Y is the peak current value of nitrite of different concentrations, meets the requirement of precision. The detection limit was 0.17. mu.M.
Note that, in fig. 1, LOD is 3Sblank/slope, where Sblank is the standard deviation of 10 blanks and the slope of the slope standard curve.
2. And (3) verifying the recovery rate:
blank labeling recovery: the sample solution to be detected is detected according to the method, and the result is as follows:
the numerical values in the above experiments are average values obtained by performing three measurements and calculating the average values.
According to the data in the table, the recovery rate of the method for preparing the graphene oxide-polyaniline-gold nanoparticle solution provided in the embodiment of the disclosure is 98-105, and the requirement of quantitative analysis precision is met.
Other embodiments of the disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. This disclosure is intended to cover any variations, uses, or adaptations of the disclosure following, in general, the principles of the disclosure and including such departures from the present disclosure as come within known or customary practice within the art to which the disclosure pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.
It will be understood that the present disclosure is not limited to the precise arrangements described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The scope of the present disclosure is limited only by the appended claims.
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| CN114740063A (en) * | 2022-02-16 | 2022-07-12 | 陕西化工研究院有限公司 | Method for detecting hydrazine by electrochemistry |
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