CN114735677A - Method for preparing platinum-polyaniline-reduced graphene oxide nano composite - Google Patents
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Abstract
The method for preparing the 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 platinum-polyaniline-reduced graphene oxide nano composite powder. According to the method for preparing the 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 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 platinum-polyaniline-reduced graphene oxide nano composite can be improved.
Description
Technical Field
The present disclosure relates to methods of preparing platinum-polyaniline-reduced graphene oxide nanocomposites.
Background
Hydrazine hydrate (N)2H4) Has important functions in various fields such as fuel cells, agriculture and the like. However, as a carcinogen, N2H4Is harmful to human health. N is a radical of hydrogen2H4Volatile and smells more irritating when inhaling N2H4Then, 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 developed2H4The analytical method of (2) is highly necessary.
At present, a number of assays have been developed for N2H4Such as high performance liquid chromatography, spectrophotometry, gas chromatography-mass spectrometry, etc. Meanwhile, electrochemical sensing methods have also received much 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 platinum-polyaniline-reduced graphene oxide nanocomposite for manufacturing the hydrazine hydrate sensor.
Disclosure of Invention
The present disclosure is directed to overcoming the disadvantages of the prior art and providing a method for preparing a platinum-polyaniline-reduced graphene oxide nanocomposite.
According to a first aspect of embodiments of the present disclosure, there is provided a method of preparing a 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 platinum-polyaniline-reduced graphene oxide nano composite powder.
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 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 of preparing a platinum-polyaniline-reduced graphene oxide nanocomposite powder includes:
s131, preparing polyaniline-graphene oxide dispersion liquid with the concentration of 0.3-0.7 mg/mL;
s132, taking 15-25mL of polyaniline-graphene oxide dispersion liquid prepared in the step S131, adding 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, centrifugally washing for a plurality of times by using ultrapure water, and drying in an oven at the temperature of 50-70 ℃ for 5-7h to prepare the platinum-polyaniline-reduced graphene oxide nano composite powder.
In one embodiment, in step S123, the oxidizing agent includes one or more of ammonium persulfate, hydrogen peroxide, and 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 dispersion with a mass concentration of 0.5mg/mL includes:
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 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 platinum-polyaniline-reduced graphene oxide nano composite, polyaniline-graphene oxide composite powder is prepared in one step by adopting an in-situ chemical polymerization method, and the preparation process is simple; in addition, the structure of the platinum-polyaniline-reduced graphene oxide nano composite in the disclosure is beneficial to maintaining the surface activity of nanoparticles, and simultaneously provides a larger specific surface area and more reaction sites, so that the sensitivity and the detection quantity range of the hydrazine sensor manufactured by the platinum-polyaniline-reduced graphene oxide nano composite can be improved.
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.
According to a first aspect of embodiments of the present disclosure, there is provided a method of preparing a 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 platinum-polyaniline-reduced graphene oxide nano composite powder.
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 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 of preparing a platinum-polyaniline-reduced graphene oxide nanocomposite powder includes:
s131, preparing polyaniline-graphene oxide dispersion liquid with the concentration of 0.3-0.7 mg/mL;
s132, taking 15-25mL of polyaniline-graphene oxide dispersion liquid prepared in the step S131, adding 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, centrifugally washing for a plurality of times by using ultrapure water, and drying in an oven at the temperature of 50-70 ℃ for 5-7h to prepare the platinum-polyaniline-reduced graphene oxide nano composite powder.
In one embodiment, in step S123, the oxidizing agent includes one or more of ammonium persulfate, hydrogen peroxide, and 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 dispersion with a mass concentration of 0.5mg/mL includes:
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 dispersion liquid with the concentration of 0.3-0.7 mg/mL.
According to the method for preparing the platinum-polyaniline-reduced graphene oxide nano composite, polyaniline-reduced graphene oxide composite powder is prepared in one step by adopting an in-situ chemical polymerization method, and the preparation process is simple; in addition, the structure of the 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 platinum-polyaniline-reduced graphene oxide nano composite can be improved.
The method of preparing the 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 water 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, then 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 then placing into an oven with the temperature of 60 ℃ to dry 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 dispersion liquid with the concentration of 0.5mg/mL, then taking 20mL of the polyaniline-graphene oxide dispersion liquid, adding 5.0mL of chloroplatinic acid solution with the concentration of 15.0mmol/L into the polyaniline-graphene oxide dispersion liquid, stirring for 10min, firstly slowly adding 2.0mL of sodium borohydride solution with the concentration of 1.9mmol/L into the solution, stirring for 90min, then 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 platinum-polyaniline-reduced graphene oxide nano composite powder.
The following examples illustrate the application scenario of the platinum-polyaniline-reduced graphene oxide nanocomposite disclosed in the present disclosure.
1. Preparing a platinum-polyaniline-reduced graphene oxide glassy carbon electrode by using the platinum-polyaniline-reduced graphene oxide nano composite in the disclosure:
firstly, adopting alumina powder with the grain size of 0.3 mu m to polish the surface of the glassy carbon electrode so that the surface of the glassy carbon electrode becomes a relatively smooth mirror surface structure, wherein the mirror surface structure can be understood as polishing the surface of the glassy carbon electrode to be similar to a mirror surface effect; then, the surface of the glassy carbon electrode is polished again by using alumina powder with the grain size of 0.05 mu m so that the surface of the glassy carbon electrode becomes a very smooth mirror surface structure, and the mirror surface structure can be understood as polishing the surface of the glassy carbon electrode to be similar to 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, 0.5g of chitosan was weighed into 100.0mL of an aqueous solution containing 1.0mL of acetic acid, and the chitosan was completely dissolved by stirring. Weighing 1.0mg of Pt/PANI/rGO and dispersing in 1mL of 0.5% chitosan solution to obtain 1mg/mL of platinum-polyaniline-reduced graphene oxide nano-composite dispersion liquid; and finally, dropping 6 mu L of the 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 as a 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 platinum-polyaniline-reduced graphene oxide glassy carbon electrode is used as a working electrode of a hydrazine sensor, phosphate buffer solution with the concentration of 0.05-0.15mol/L, pH of 5.5-8.0 is used as supporting electrolyte of 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 values are 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 electrochemical detection of hydrazine hydrate 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-1.951 +32.78X, the detection limit is 3.3 μmol, and the linear correlation coefficient R is 0.9978, which meets the requirement of precision, wherein X is the concentration of hydrazine in mol/L, Y is the peak current value of hydrazine in different concentrations in μ a, the detection limit is the minimum concentration or minimum amount of the substance to be detected that can be detected from the sample by a specific analysis method within a given confidence, and the detection limit is 3.3 μmol, which is the minimum concentration or minimum amount of the substance to be detected that can be detected from the sample by a specific analysis method within a given confidence.
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:
table 1 blank spiked recovery: the sample solution to be detected is detected according to the method, and the result is as follows:
and a standard recovery method is adopted to perform a sample test on the platinum-polyaniline-reduced graphene oxide nano glassy carbon electrode. Different concentrations of N2H4The results were shown in Table 1, after adding to tap water. Through experiments, N is found2H4The recovery rate range of (1) is 98.0% -104.0%. This indicates that the substance pair in tap water detects N2H4The influence of (a) is small, and the electrochemical sensor can be applied to N in a sample2H4Detection of (3).
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, N2H4The recovery rate range of (A) is 99.3% -104.0%. This indicates that the substance pair in tap water detects N2H4The influence of (a) is small, and the electrochemical sensor can be applied to N in a sample2H2Detection 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 platinum-polyaniline-reduced graphene oxide nanocomposite is characterized by comprising the following steps:
s11, preparing graphene oxide powder;
s12, preparing polyaniline-graphene oxide composite powder;
s13, preparing platinum-polyaniline-reduced graphene oxide nano composite powder.
2. The method of preparing a 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 preparing platinum-polyaniline-reduced graphene oxide nanocomposite as claimed in claim 1, wherein in step S12, polyaniline-graphene oxide composite powder is prepared using in-situ chemical polymerization.
4. The method for preparing platinum-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 for preparing platinum-polyaniline-reduced graphene oxide nanocomposite powder according to claim 1, wherein in step S13, the method for preparing platinum-polyaniline-reduced graphene oxide nanocomposite powder comprises:
s131, preparing polyaniline-graphene oxide dispersion liquid with the concentration of 0.3-0.7 mg/mL;
s132, taking 15-25mL of polyaniline-graphene oxide dispersion liquid prepared in the step S131, adding 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, centrifugally washing for a plurality of times by using ultrapure water, and drying in an oven at the temperature of 50-70 ℃ for 5-7h to prepare the 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, and dichromate.
7. The method of preparing the platinum-polyaniline-reduced graphene oxide nanocomposite as claimed in claim 4, wherein in the step S121, the preparing the graphene oxide solution with a concentration of 0.3-0.7mg/mL 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 the platinum-polyaniline-reduced graphene oxide nanocomposite according to claim 5, wherein in the step S131, the preparing the polyaniline-graphene oxide 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 a polyaniline-graphene oxide dispersion liquid with the concentration of 0.3-0.7 mg/mL.
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| US20170113934A1 (en) * | 2009-08-17 | 2017-04-27 | Carnegie Mellon University | Heteroatom-enriched partially-graphitic nano-carbons |
| CN102350372A (en) * | 2011-07-12 | 2012-02-15 | 南昌大学 | Preparation method of polyaniline/graphene controllable load platinum nanoparticles |
| CN113813945A (en) * | 2021-09-30 | 2021-12-21 | 宁德师范学院 | Three-dimensional space network graphene-based polyaniline/PtAg composite catalyst and preparation method thereof |
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