CN114890412A - Method for preparing gold platinum-polyaniline-reduced graphene oxide nano composite - Google Patents
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- CN114890412A CN114890412A CN202210142206.2A CN202210142206A CN114890412A CN 114890412 A CN114890412 A CN 114890412A CN 202210142206 A CN202210142206 A CN 202210142206A CN 114890412 A CN114890412 A CN 114890412A
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Abstract
The method for preparing the gold platinum-polyaniline-reduced graphene oxide nano composite comprises the following steps: s11, preparing graphene oxide powder; s12, preparing polyaniline-graphene oxide composite powder; s13, preparing gold platinum-polyaniline-reduced graphene oxide nano composite powder. The gold platinum-polyaniline-reduced graphene oxide nano composite prepared in the disclosure is a bimetallic composite material, and the electrocatalytic activity of the gold platinum-polyaniline-reduced graphene oxide nano composite is higher, so that the linear range of a hydrazine sensor manufactured by the gold platinum-polyaniline-reduced graphene oxide nano composite can be widened by 2 orders of magnitude, the sensitivity can be improved by 3.9 times, and the detection limit can be reduced by 19.4 times.
Description
Technical Field
The present disclosure relates to a method of preparing a gold platinum-polyaniline-reduced graphene oxide nanocomposite.
Background
Hydrazine hydrate (N) 2 H 4 ) In the fuelThe method plays an important role in a plurality of fields such as batteries, agriculture and the like. However, as a carcinogen, N 2 H 4 Endangering the health of the human body. N is a radical of 2 H 4 Volatile and smells more irritating when inhaling N 2 H 4 Then, the medicine will cause harm to the lung, kidney, liver, central nervous system, reproductive system and the like of the organism. Thus, the detection N was developed 2 H 4 The analytical method of (2) is highly necessary.
At present, a number of assays have been developed for N 2 H 4 Methods such as high performance liquid chromatography, spectrophotometry, gas chromatography-mass spectrometry, and the like. Meanwhile, electrochemical sensing methods have also received great attention because of their advantages such as good detection performance, simplicity and low cost. Therefore, there is an urgent need to develop a hydrazine hydrate method which is simple, sensitive, highly selective, economical, and suitable for environmental monitoring, food industry, and clinical diagnosis. Therefore, the establishment of an accurate and effective hydrazine hydrate detection method has important application value and practical significance, and the premise to establish the accurate and effective hydrazine hydrate detection method is how to prepare the gold platinum-polyaniline-reduced graphene oxide nano composite for manufacturing the hydrazine hydrate sensor.
Disclosure of Invention
The purpose of the present disclosure is to overcome the shortcomings of the prior art and provide a method for preparing a gold platinum-polyaniline-reduced graphene oxide nanocomposite.
According to a first aspect of embodiments of the present disclosure, there is provided a method for preparing a gold platinum-polyaniline-reduced graphene oxide nanocomposite, the method comprising the steps of:
s11, preparing graphene oxide powder;
s12, preparing polyaniline-graphene oxide composite powder;
s13, preparing gold platinum-polyaniline-reduced graphene oxide nano composite powder.
In one embodiment, in step S11, the method for 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 S12, an in-situ chemical polymerization method is used to prepare polyaniline-graphene oxide composite powder.
In one embodiment, in step S12, the method for preparing polyaniline-graphene oxide composite powder by using in-situ chemical polymerization includes:
s121, preparing a graphene oxide solution with the concentration of 0.3-0.7 mg/mL;
s122, taking 15-25mL of the graphene oxide solution prepared in the step S121, dropwise adding 35-45 mu L of aniline solution into the graphene oxide solution, and violently stirring in an ice bath for 25-35 min;
s123, slowly adding 4.3-5.3mL of 0.8-1.2mol/L hydrochloric acid solution into the solution prepared in the step S122, wherein the hydrochloric acid solution contains 0.030-0.042g of oxidant, stirring at room temperature for 20-28h, centrifuging, washing with secondary distilled water for several times, and drying in an oven at 50-70 ℃ for 2.5-3.5h to prepare polyaniline-graphene oxide composite powder.
In one embodiment, in step S13, the method for preparing the gold platinum-polyaniline-reduced graphene oxide nanocomposite powder includes:
s131, preparing polyaniline-graphene oxide nanocomposite dispersion liquid with the concentration of 0.3-0.7 mg/mL;
s132, taking 15-25mL of the polyaniline-graphene oxide nanocomposite dispersion liquid prepared in the step S131, adding 3.0-7.0mL of chloroauric acid solution with the concentration of 12-18.0mmol/L and 3.0-7.0mL of chloroplatinic acid solution with the concentration of 12-18.0mmol/L, and stirring for 7-13 min;
s133, slowly adding 1.5-2.5mL of 1.6-2.2mmol/L sodium borohydride solution into the solution prepared in the step S132, stirring for 80-100min, centrifuging, washing for several times by using secondary distilled water, and drying in an oven at 50-70 ℃ for 5-7h to prepare the gold platinum-polyaniline-reduced graphene oxide nano composite powder.
In one embodiment, in step S123, the oxidizing agent includes one or any of ammonium persulfate, hydrogen peroxide, or dichromate.
In one embodiment, in step S121, the preparing the graphene oxide solution with a concentration of 0.3-0.7mg/mL includes:
and (3) adding 3-7mg of the graphene oxide powder prepared in the step S11 into 8-12mL of deionized water, and performing ultrasonic dissolution to form a graphene oxide solution with the concentration of 0.3-0.7 mg/mL.
In one embodiment, in step S131, the preparing the polyaniline-graphene oxide nanocomposite dispersion with a mass concentration of 0.5mg/mL includes:
and (3) adding 3-7mg of polyaniline-graphene oxide compound powder prepared in the step S12 into 8-12mL of deionized water, and performing ultrasonic dissolution to form polyaniline-graphene oxide nano compound dispersion liquid with the concentration of 0.3-0.7 mg/mL.
The implementation of the present disclosure includes the following technical effects:
according to the method for preparing the gold platinum-polyaniline-reduced graphene oxide nano composite, the gold platinum-polyaniline-reduced graphene oxide nano composite powder is prepared by adopting an in-situ chemical polymerization method, and the preparation process is simple; in addition, the structure of the gold platinum-polyaniline-reduced graphene oxide nano composite in the disclosure is beneficial to maintaining the surface activity of nano particles, and simultaneously provides a larger specific surface area and more reaction sites, so that the detection sensitivity and the detection quantity range of a hydrazine sensor manufactured by the gold platinum-polyaniline-reduced graphene oxide nano composite can be improved. Moreover, the gold platinum-polyaniline-reduced graphene oxide nanocomposite prepared in the disclosure is a bimetallic composite material, and the electrocatalytic activity of the composite material is higher, so that the linear range of a hydrazine sensor manufactured by the gold platinum-polyaniline-reduced graphene oxide nanocomposite can be widened by 2 orders of magnitude, the sensitivity can be improved by 3.9 times, and the detection limit can be reduced by 19.4 times.
Drawings
FIG. 1 is a fitted standard graph 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 do not 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.
According to a first aspect of embodiments of the present disclosure, there is provided a method for preparing a gold platinum-polyaniline-reduced graphene oxide nanocomposite, the method comprising the steps of:
s11, preparing graphene oxide powder;
s12, preparing polyaniline-graphene oxide composite powder;
s13, preparing gold platinum-polyaniline-reduced graphene oxide nano composite powder.
In one embodiment, in step S11, the method for 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 S12, an in-situ chemical polymerization method is used to prepare polyaniline-graphene oxide composite powder.
In one embodiment, in step S12, the method for preparing polyaniline-graphene oxide composite powder by using in-situ chemical polymerization includes:
s121, preparing a graphene oxide solution with the concentration of 0.3-0.7 mg/mL;
s122, taking 15-25mL of the graphene oxide solution prepared in the step S121, dropwise adding 35-45 mu L of aniline solution into the graphene oxide solution, and violently stirring in an ice bath for 25-35 min;
s123, slowly adding 4.3-5.3mL of 0.8-1.2mol/L hydrochloric acid solution into the solution prepared in the step S122, stirring at room temperature for 20-28h, centrifuging, washing with secondary distilled water for several times, and drying in an oven at 50-70 ℃ for 2.5-3.5h to obtain polyaniline-graphene oxide composite powder.
In one embodiment, in step S13, the method for preparing the gold platinum-polyaniline-reduced graphene oxide nanocomposite powder includes:
s131, preparing polyaniline-graphene oxide nanocomposite dispersion liquid with the concentration of 0.3-0.7 mg/mL;
s132, taking 15-25mL of the polyaniline-graphene oxide nanocomposite dispersion liquid prepared in the step S131, adding 3.0-7.0mL of chloroauric acid solution with the concentration of 12-18.0mmol/L and 3.0-7.0mL of chloroplatinic acid solution with the concentration of 12-18.0mmol/L, and stirring for 7-13 min;
s133, slowly adding 1.5-2.5mL of 1.6-2.2mmol/L sodium borohydride solution into the solution prepared in the step S132, stirring for 80-100min, centrifuging, washing for several times by using secondary distilled water, and drying in an oven at 50-70 ℃ for 5-7h to prepare the gold platinum-polyaniline-reduced graphene oxide nano composite powder.
In one embodiment, in step S123, the oxidizing agent includes one or any of ammonium persulfate, hydrogen peroxide, or dichromate.
In one embodiment, in step S121, the preparing the graphene oxide solution with a concentration of 0.3-0.7mg/mL includes:
and (3) adding 3-7mg of the graphene oxide powder prepared in the step S11 into 8-12mL of deionized water, and performing ultrasonic dissolution to form a graphene oxide solution with the concentration of 0.3-0.7 mg/mL.
In one embodiment, in step S131, the preparing the polyaniline-graphene oxide nanocomposite dispersion with a mass concentration of 0.5mg/mL includes:
and (3) adding 3-7mg of polyaniline-graphene oxide compound powder prepared in the step S12 into 8-12mL of deionized water, and performing ultrasonic dissolution to form polyaniline-graphene oxide nano compound dispersion liquid with the concentration of 0.3-0.7 mg/mL.
According to the method for preparing the gold platinum-polyaniline-reduced graphene oxide nano composite, polyaniline-graphene oxide composite powder is prepared by adopting an in-situ chemical polymerization method, so that the preparation process is simple; in addition, the structure of the gold platinum-polyaniline-reduced graphene oxide nano composite in the disclosure is beneficial to maintaining the surface activity of nano particles, and simultaneously provides a larger specific surface area and more reaction sites, so that the detection sensitivity and the detection quantity range of a hydrazine sensor manufactured by the gold platinum-polyaniline-reduced graphene oxide nano composite can be improved. Moreover, the gold platinum-polyaniline-reduced graphene oxide nanocomposite prepared in the disclosure is a bimetallic composite material, and the electrocatalytic activity of the composite material is higher, so that the linear range of a hydrazine sensor manufactured by the gold platinum-polyaniline-reduced graphene oxide nanocomposite can be widened by 2 orders of magnitude, the sensitivity can be improved by 3.9 times, and the detection limit can be reduced by 19.4 times.
The method for preparing the gold platinum-polyaniline-reduced graphene oxide nanocomposite according to the present disclosure will be specifically described below with specific examples.
Firstly, graphite powder is used as a raw material, and an ultrasonic stripping dispersion method is adopted to synthesize graphene oxide powder in an ultrasonic bath; then taking 5mg of the graphene oxide powder, performing ultrasonic dispersion and dissolution by using 10mL of deionized water to form a graphene oxide solution with the concentration of 0.5mg/mL, then taking 20mL of the graphene oxide solution, dropwise adding 40 mu L of aniline solution into the graphene oxide solution, violently stirring in an ice bath for 30min, slowly adding 4.8mL of 1.0mol/L hydrochloric acid solution containing 0.036g of ammonium persulfate, stirring at room temperature for 24h, performing centrifugal treatment, washing with secondary distilled water for three times, and drying in an oven at the temperature of 60 ℃ for 3h to form polyaniline-graphene oxide composite powder; and finally, taking 5mg of polyaniline-graphene oxide composite powder, performing ultrasonic dispersion and dissolution by using 10mL of deionized water to form polyaniline-graphene oxide nano composite dispersion liquid with the concentration of 0.5mg/mL, then taking 20mL of the polyaniline-graphene oxide nano composite dispersion liquid, adding 5.0mL of chloroauric acid solution with the concentration of 15.0mmol/L and 5.0mL of chloroplatinic acid solution with the concentration of 15.0mmol/L into the polyaniline-graphene oxide nano composite dispersion liquid, stirring for 10min, slowly adding 2.0mL of sodium borohydride solution with the concentration of 1.9mmol/L into the polyaniline-graphene oxide nano composite dispersion liquid, stirring for 90min, performing centrifugal treatment, washing for three times by using secondary distilled water, drying in an oven with the temperature of 60 ℃ for 6h, and preparing the gold platinum-polyaniline-reduced graphene oxide nano composite powder.
The following examples illustrate the application scenario of the gold platinum-polyaniline-reduced graphene oxide nanocomposite disclosed in the present disclosure.
1. Preparing a gold platinum-polyaniline-reduced graphene oxide glassy carbon electrode by using the gold platinum-polyaniline-reduced graphene oxide nanocomposite disclosed by the invention:
firstly, the surface of a glassy carbon electrode is polished by adopting alumina powder with the particle size of 0.3 mu m, so that the surface of the glassy carbon electrode is changed into a relatively smooth mirror surface structure, and the mirror surface structure can be understood as polishing the surface of the glassy carbon electrode into a mirror surface-like effect; secondly, polishing the surface of the glassy carbon electrode by using alumina powder with the particle size of 0.05 mu m again to ensure that the surface of the glassy carbon electrode becomes a very smooth mirror surface structure, wherein the mirror surface structure can be understood as polishing the surface of the glassy carbon electrode into a mirror surface effect; then, repeatedly ultrasonically cleaning the surface of the glassy carbon electrode by using a mixed solution of secondary distilled water and ethanol, wherein the volume ratio of the secondary distilled water to the ethanol is 1: 1; then adding 1mg of the prepared gold platinum-polyaniline-reduced graphene oxide nanocomposite powder into 1mL of chitosan solution with the mass fraction of 0.5% for ultrasonic dispersion to obtain 1mg/mL of gold platinum-polyaniline-reduced graphene oxide nanocomposite dispersion liquid; and finally, dripping 6 mu L of the gold platinum-polyaniline-reduced graphene oxide nano composite dispersion liquid on the surface of a glassy carbon electrode with a mirror surface structure to modify the glassy carbon electrode, and naturally airing at room temperature for use, wherein the modified electrode is called a gold platinum-polyaniline-reduced graphene oxide glassy carbon electrode.
2. Fitting a standard curve:
an Ag/AgCl electrode is used as a reference electrode, a Pt electrode is used as a counter electrode, a gold platinum-polyaniline-reduced graphene oxide glassy carbon electrode is used as a working electrode of a hydrazine sensor, a phosphate buffer solution with the concentration of 0.05-0.15mol/L, pH of 5.5-8.0 is used as a supporting electrolyte for electrochemical detection, peak current values of different concentrations are detected, the concentration of a hydrazine standard solution is used as a horizontal coordinate, the peak current value is used as a vertical coordinate, and a standard curve is fitted. The fitted standard curve is shown in fig. 1.
3. And detecting the hydrazine hydrate in the solution to be detected according to the standard curve.
The reliability verification of the hydrazine hydrate by adopting electrochemical detection provided by the disclosure comprises the following steps:
1. and (3) verifying linear correlation:
the standard curve obtained in the embodiments of the present disclosure as shown in fig. 1 is plotted by origin 8.0 software, and the formula of the fitted standard curve is: current value and N 2 H 4 The concentrations in the range of 0.5 mu mol-0.38 mmol, 0.38 mmol-1.28 mmol and 1.28 mmol-4.78 mmol respectively show better linear relations, the linear equations are respectively I1-69.93 + 23.41. C1, I2-22.79 + 126.7. C2, I3-0.91 + 32.72. C3, the detection limit is 0.17 mu mol. L-1 (S/N-3), wherein, I represents current, the unit mu A thereof, C represents N, and the unit thereof represents N 2 H 4 Concentration in mmol/L, I1 is N 2 H 4 A current value corresponding to a concentration of 0.5. mu. mol to 0.38mmol, I2 is N 2 H 4 A current value corresponding to a concentration of 0.38mmol to 1.28mmol, I3 is N 2 H 4 The concentration is a current value corresponding to 1.28 mmol-4.78 mmol, the detection limit is the minimum concentration or the minimum amount of the substance to be detected which can be detected from the sample by a specific analysis method within a given confidence coefficient, and S/N is 3, which means that the signal-to-noise ratio is 3.
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:
and (3) carrying out a sample test on the gold platinum-polyaniline-reduced graphene oxide nano glassy carbon electrode by adopting a standard recovery method. Different concentrations of N 2 H 4 The results were shown in Table 1, after adding to tap water. Through experiments, N is found 2 H 4 The recovery rate range of (1) is 98.0% -104.0%. This indicates that the substance pair in tap water detects N 2 H 4 The influence of (a) is small, and the electrochemical sensor can be applied to N in a sample 2 H 4 Detection of (3).
TABLE 1N in tap water 2 H 4 Result of detection of
In Table 1, a is the average of the results of 3 measurements, and b is the relative standard deviation.
The numerical values in the above experiments are average values obtained by performing three measurements and calculating the average values.
From the data in the above table, N 2 H 4 The recovery rate range of (1) is 98.0% -104.0%. This indicates that the substance pair in tap water detects N 2 H 4 The effect of (a) is small, and the electrochemical sensor can be applied to N in a sample 2 H 4 Detection of (3).
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.
Claims (8)
1. A method for preparing a gold platinum-polyaniline-graphene oxide nano composite is characterized by comprising the following steps:
s11, preparing graphene oxide powder;
s12, preparing polyaniline-graphene oxide composite powder;
s13, preparing gold platinum-polyaniline-reduced graphene oxide nano composite powder.
2. The method of preparing a gold platinum-polyaniline-reduced graphene oxide nanocomposite as claimed in claim 1, wherein in step S11, the method of preparing graphene oxide powder comprises:
graphite powder is used as a raw material, and an ultrasonic stripping dispersion method is adopted to synthesize graphene oxide in an ultrasonic bath.
3. The method of claim 1, wherein in step S12, polyaniline-graphene oxide composite powder is prepared by in-situ chemical polymerization.
4. The method for preparing Au-Pt-polyaniline-reduced-graphene oxide nanocomposite as claimed in claim 3, wherein in step S12, the method for preparing polyaniline-graphene oxide composite powder by in-situ chemical polymerization comprises:
s121, preparing a graphene oxide solution with the concentration of 0.3-0.7 mg/mL;
s122, taking 15-25mL of the graphene oxide solution prepared in the step S121, dropwise adding 35-45 mu L of aniline solution into the graphene oxide solution, and violently stirring in an ice bath for 25-35 min;
s123, slowly adding 4.3-5.3mL of 0.8-1.2mol/L hydrochloric acid solution into the solution prepared in the step S122, wherein the hydrochloric acid solution contains 0.030-0.042g of oxidant, stirring at room temperature for 20-28h, centrifuging, washing with secondary distilled water for several times, and drying in an oven at 50-70 ℃ for 2.5-3.5h to prepare polyaniline-graphene oxide composite powder.
5. The method of preparing a gold platinum-polyaniline-reduced graphene oxide nanocomposite powder according to claim 1, wherein in step S13, the method of preparing a gold platinum-polyaniline-reduced graphene oxide nanocomposite powder comprises:
s131, preparing polyaniline-graphene oxide nanocomposite dispersion liquid with the concentration of 0.3-0.7 mg/mL;
s132, taking 15-25mL of the polyaniline-graphene oxide nanocomposite dispersion liquid prepared in the step S131, adding 3.0-7.0mL of chloroauric acid solution with the concentration of 12-18.0mmol/L and 3.0-7.0mL of chloroplatinic acid solution with the concentration of 12-18.0mmol/L, and stirring for 7-13 min;
s133, slowly adding 1.5-2.5mL of 1.6-2.2mmol/L sodium borohydride solution into the solution prepared in the step S132, stirring for 80-100min, centrifuging, washing for several times by using secondary distilled water, and drying in an oven at 50-70 ℃ for 5-7h to prepare the gold platinum-polyaniline-reduced graphene oxide nano composite powder.
6. The method of claim 4, wherein in step S123, the oxidant comprises one or more of ammonium persulfate, hydrogen peroxide, or dichromate.
7. The method of claim 4, wherein the preparing the graphene oxide solution with the concentration of 0.3-0.7mg/mL in step S121 comprises:
and (3) adding 3-7mg of the graphene oxide powder prepared in the step S11 into 8-12mL of deionized water, and performing ultrasonic dissolution to form a graphene oxide solution with the concentration of 0.3-0.7 mg/mL.
8. The method for preparing a gold platinum-polyaniline-reduced graphene oxide nanocomposite as claimed in claim 5, wherein in the step S131, the preparing of the polyaniline-graphene oxide nanocomposite dispersion liquid with the mass concentration of 0.5mg/mL comprises:
and (3) adding 3-7mg of polyaniline-graphene oxide composite powder prepared in the step S12 into 8-12mL of deionized water, and performing ultrasonic dissolution to form polyaniline-graphene oxide nano composite dispersion liquid with the concentration of 0.3-0.7 mg/mL.
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