CN111007122A - Three-dimensional flower-like nano composite material and preparation method and application thereof - Google Patents
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Abstract
The invention provides a three-dimensional flower-like nano composite material, a preparation method and application thereof, wherein the composite material is NiO/PDDA-RGO, and the preparation method is to obtain NiO synthesized by calcining PDDA-RGO and hydrothermal reaction by an ultrasonic-assisted method. The reduced graphene oxide in the composite material is used as a carrier of NiO, so that the problem of poor conductivity of NiO is solved, the adsorption characteristic of an analyte is improved to enhance the electrochemical performance, and the composite material is an excellent electrode modification material. The NiO/PDDA-RGO composite material is modified on the surface of an electrode, and electrochemical sensing is constructed for non-enzyme nitrite detection. The method overcomes the technical problems of long identification time, complexity, high cost, low sensitivity, unobvious identification effect and the like in the prior art, can realize high-sensitivity and high-selectivity detection on nitrite in a complex environment, and has a very good application prospect in the analysis fields of environment, food and the like.
Description
Technical Field
The invention relates to electrochemical detection of a nano composite material, in particular to a three-dimensional flower-shaped nano composite material, a preparation method thereof and application of the material in nitrite detection.
Background
Nitrite (NO)2-) Are common important ingredients in coloring agents, food preservatives and agricultural fertilizers. However, NO2-As well as excessive use of toxic inorganic pollutants, long-term accumulation and non-treatment of large amounts of emissions can cause significant damage to environmental systems and human health, even nitrite can interact with amines and amides to produce carcinogenic N-nitrosamines, leading to potential cancer risks and "blue infant syndrome". In addition, nitrite can react irreversibly with hemoglobin in human blood to produce methemoglobin, which reduces the oxygen transport capacity of the blood. The world health organization has reported that the lethal dose ranges from 8.7 μ M to 28.3 μ M of NO2-. Therefore, there is a great need to develop reliable, sensitive and accurate methods for detecting NO2-. To date, different analytical techniques have been successfully applied to the detection of nitrite such as chemiluminescence, fluorescence, colorimetric analysis, chromatography, spectrophotometry, capillary electrophoresis and electrochemical methods. Electrochemical sensors, especially enzyme-free sensors, are of great interest due to their ease of operation, on-site monitoring, low cost and high sensitivity, which can overcome the disadvantages of enzymatic methods such as cumbersome immobilization procedures, instability and high cost. In order to improve the performance of the sensor, it is important to find materials that meet the above requirements.
Disclosure of Invention
The invention aims to provide a three-dimensional flower-like nano composite NiO/PDDA-RGO (nickel oxide-PDDA-reduced graphene oxide) and a preparation method thereof, and the composite material is used for detecting nitrite, so as to solve the technical problems of long identification time, complexity, high cost, low sensitivity, unobvious identification effect and the like in the prior art.
According to the invention, the three-dimensional flower-shaped NiO is compounded with the PDDA-RGO with good water solubility, and the reduced graphene oxide in the composite material is used as a carrier of the NiO, so that the problem of poor conductivity of the NiO is solved, the adsorption characteristic of an analyte is improved to enhance the electrochemical performance, and the composite material is an excellent electrode modification material. The NiO/PDDA-RGO composite material is modified on the surface of an electrode, and electrochemical sensing is constructed for nitrite enzyme-free detection. The method can realize high-sensitivity and high-selectivity detection of nitrite in a complex environment, and has a very good application prospect in the analysis fields of environment, food and the like.
The invention is realized by the following technical scheme:
a method for preparing a three-dimensional flower-like nano composite NiO/PDDA-RGO comprises the following steps:
1) preparation of PDDA-RGO:
carrying out ultrasonic treatment on 15-50mg of graphene oxide in 15-25mL of deionized water for 0.5-3h (preferably 3h) to obtain graphene oxide dispersion liquid, and then placing the graphene oxide dispersion liquid in a container; then, taking 5-10.0 mL of graphene oxide dispersion liquid with the concentration of 1.0-2.0 mg/mL into a reaction bottle, adding 50.0-60.0 mu L of PDDA with the concentration of 8.0-12.0 wt%, fully stirring and uniformly mixing, and then adjusting the pH value to 9-10.0 by using concentrated ammonia water; adding 40.0-55.0 mu L of 80% hydrazine hydrate, stirring vigorously, placing the reaction bottle in a 50-80 ℃ water bath kettle, heating for 3-4h, cooling to room temperature, washing and drying the synthesized material to obtain PDDA-RGO;
2) preparing three-dimensional flower-like NiO:
adding 0.06-0.07g NH4F，0.2-0.3g Ni(NO3)2.6H2O, 0.3 to 0.5g of urea, was added to a mixed solution of 20mL of distilled water and 0.635mL of ethylene glycol in this order, the solution was stirred uniformly for 0.5 to 1h (preferably 1h), and then the solution was transferred to a 50mL reaction vessel and reacted at 130 ℃ to 150 ℃ for 8 to 10h (preferably 10 h). And (3) centrifugally washing the light blue liquid obtained after the reaction is finished, and drying at 80 ℃ for 2h to obtain light blue powder. Placing the crucible containing the powder in a muffle furnace at 5 deg.C for min-1Heating to react for 2-3h (preferably 3h) at the temperature rising speed of 380-400 ℃ (preferably 400 ℃), thus obtaining the three-dimensional flower-shaped NiO;
3) preparing a three-dimensional flower-like nano composite NiO/PDDA-RGO:
firstly, 10-30mg of PDDA-RGO synthesized in the step 1) is subjected to ultrasonic treatment in 10-30mL of distilled water for 0.5-1h (preferably 0.5h), 1.25-20mg of NiO is added after the PDDA-RGO is completely and uniformly dispersed, and ultrasonic treatment is carried out at room temperature for 2-3h (preferably 3h), so as to obtain the three-dimensional flower-shaped nano composite NiO/PDDA-RGO.
The three-dimensional flower-like nano composite NiO/PDDA-RGO prepared by the method can be used for detecting nitrite.
The preparation method of the NiO/PDDA-RGO modified electrode comprises the following steps:
polishing the surface of the naked GCE with 0.05 mu m of alumina particles, carefully flushing with ultrapure water and ethanol until a mirror surface is obtained and drying, transferring 6-8 mu L (preferably 8 mu L) of prepared NiO/PDDA-RGO to the surface of a Glassy Carbon Electrode (GCE), and fully baking under an infrared lamp to obtain the NiO/PDDA-RGO modified electrode (NiO/PDDA-RGO/GCE).
A method for detecting nitrite by using a three-dimensional flower-like nano composite material NiO/PDDA-RGO comprises the following steps:
preparing a series of sodium nitrite standard solutions with different concentrations, taking the prepared NiO/PDDA-RGO/GCE as a working electrode, a platinum wire electrode as a counter electrode and a silver-silver chloride electrode as a reference electrode, placing the three electrodes in a solution taking 0.1M phosphate buffer solution (pH 5) as electrolyte, recording peak currents corresponding to the sodium nitrite with different concentrations by adopting a current-time method, and drawing a standard curve of the current versus the concentration according to the peak current value and the concentration of the sodium nitrite in the corresponding standard solution.
Compared with the prior art, the invention has the following beneficial effects: the three-dimensional flower-like nano composite NiO/PDDA-RGO prepared by the method has the characteristics of excellent adsorption and catalysis performance, large specific surface area, good biocompatibility, excellent electronic conductivity, more active sites and the like, can be used for sensitive and rapid detection of nitrite, and shows good anti-interference capability, excellent stability and repeatability.
The electrochemical analysis method adopted by the invention has higher sensitivity, the lowest detection limit reaches 0.98 mu M, the method has the advantages of cheap and portable instruments, simple method and convenient operation, and the constructed electrochemical sensing platform has potential application value in the field detection of nitrite in the analysis fields of environment, food and the like.
Drawings
FIG. 1 is a scanning electron micrograph of NiO;
FIG. 2 is an infrared spectrum of NiO, NiO/PDDA-RGO and PDDA-RGO;
FIG. 3 is a cyclic voltammogram of bare electrode (GCE), NiO/GCE, PDDA-RGO/GCE, and NiO/PDDA-RGO/GCE in 0.1M PBS (pH 5) containing 1mM sodium nitrite;
FIG. 4(A) is a time-current diagram of the current as a function of the concentration of sodium nitrite when NiO/PDDA-RGO/GCE is used for detecting sodium nitrite; (B) a current versus time linear plot;
FIG. 5 is a time-current plot of NiO/PDDA-RGO/GCE versus sodium nitrite and other interference detection.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the present invention.
Example 1
A method for preparing a three-dimensional flower-like nano composite NiO/PDDA-RGO comprises the following steps:
1) preparation of PDDA-RGO:
and (3) carrying out ultrasonic treatment on 20mg of graphene oxide in 20mL of deionized water for 3h to obtain a graphene oxide dispersion solution, and then placing the graphene oxide dispersion solution in a container. Then, 10mL of graphene oxide dispersion liquid with the concentration of 1.0mg/mL is taken out to be placed in a reaction bottle, 50.0 mu L of PDDA with the concentration of 10.0 wt% is added to be fully stirred and uniformly mixed, and then the pH value is adjusted to be 10.0 through strong ammonia water; then adding 50.0 μ L of 80% hydrazine hydrate, stirring vigorously, placing the reaction bottle in a 60 deg.C water bath, heating for 4h, cooling to room temperature, washing the synthesized material, and drying to obtain PDDA-RGO.
2) Preparing three-dimensional flower-like NiO:
0.066g of NH4F, 0.26g of Ni (NO3)2.6H2O and 0.35g of urea are sequentially added to a mixed solution of 20mL of distilled water and 0.635mL of ethylene glycol, the solution is uniformly stirred for 1H, and then the solution is transferred to a 50mL reaction kettle and reacted at 130 ℃ for 10H. Centrifuging the light blue liquid obtained after the reaction, washing at 80 deg.CDrying for 2h gave a pale blue powder. Placing the crucible containing the powder in a muffle furnace at 5 deg.C for min-1The temperature is raised at the speed of 400 ℃ and the reaction is carried out for 3 h. And obtaining the three-dimensional flower-shaped NiO.
3) Preparing a three-dimensional flower-like nano composite NiO/PDDA-RGO:
firstly, 10mg of PDDA-RGO powder synthesized in the step 1) is subjected to ultrasonic treatment in 10mL of distilled water for 0.5h, 7.5mg of NiO is added after the PDDA-RGO powder is completely and uniformly dispersed, and the three-dimensional flower-shaped NiO/PDDA-RGO nano composite material is obtained after ultrasonic treatment at room temperature for 3 h. Fig. 1 is a scanning electron micrograph of NiO, which shows that it has a flower-like structure of mesopores and is composed of a combination of overlapping nanosheets. FIG. 2 is an infrared spectrum of NiO, NiO/PDDA-RGO and PDDA-RGO at 3423.48cm-1The peak observed at (1) for O-H, C ═ O (1746 cm)-1)，C-O(1183.67cm-1) And C-OH (1399.54 cm)-1) Peaks were also observed. 418.96cm-1And 1632.53cm-1The nearby broad absorption is attributed to Ni-O vibration absorption and O-H tensile deformation. The maximum absorption peak is 3465cm-1The nearby broad absorption region should be derived from-OH. In the NiO/PDDA-RGO infrared spectrogram, the characteristic peaks of PDDA-RGO and NiO can also be observed in the composite material, which indicates that the composite material NiO/PDDA-rGO is successfully synthesized.
Example 2
The establishment and anti-interference experiment of the method for detecting nitrite by using the three-dimensional flower-shaped nano composite NiO/PDDA-RGO are as follows:
1) the bare GCE surface was polished with 0.05 μm alumina particles and carefully rinsed with ultrapure water and ethanol until a mirror surface was obtained and dried, and 8 μ L of the NiO/PDDA-RGO composite prepared in example 1 was transferred to be applied dropwise onto the surface of a Glassy Carbon Electrode (GCE) and sufficiently baked under an infrared lamp to obtain a NiO/PDDA-RGO modified electrode (NiO/PDDA-RGO/GCE). As a control, NiO/GCE and PDDA-RGO/GCE were prepared in the same manner.
2) GCE, NiO/GCE, PDDA-RGO/GCE and NiO/PDDA-RGO/GCE were immersed in a solution of 1mM sodium nitrite in 0.1M PBS (pH 5), and the peak currents for the different electrodes were recorded using cyclic voltammetry. As shown in FIG. 3, it can be seen that the electrodes are more numerous than the othersNiO/PDDA-RGO/GCE vs. NaNO2The catalyst shows excellent electrooxidation activity, has good catalytic activity and excellent conductivity due to good synergistic effect of NiO and PDDA-RGO, and can accelerate electron transfer.
3) Preparing sodium nitrite standard solutions (10) with different concentrations-4-10-2mol L-1) The prepared NiO/PDDA-RGO/GCE is used as a working electrode, a platinum wire electrode is used as a counter electrode, a silver-silver chloride electrode is used as a reference electrode, the three electrodes are placed in a solution taking 0.1M phosphate buffer (pH 5) as an electrolyte, peak currents corresponding to different concentrations of sodium nitrite are recorded by a current-time method, and an i-t curve of the peak currents along with the change of the concentration of the sodium nitrite is shown in a graph 4 (A). A standard curve for sodium nitrite analysis was plotted according to the peak current change value and the corresponding concentration, as shown in fig. 4 (B). As can be seen from the graph (A), when sodium nitrite was added, the reaction was rapid and reached a steady state within 5s, and the current was also increased as the concentration was increased. The graph (B) shows that the current and the concentration of the sodium nitrite are in good linear relation, and the linear fitting equation of the sodium nitrite detection is Ip＝0.00735C+0.1259,R20.9983, the sensor has a broad linear range of 5 μ M to 8mM, with a low detection limit of 0.98 μ M.
4) Selectivity of the electrode: respectively adding a sodium nitrite solution and an interferent solution with the concentration of 50 times into a three-electrode test system, wherein the interferents are respectively calcium chloride, sodium chloride, zinc sulfate, glucose, ammonium fluoride, potassium bromide, magnesium sulfate, ascorbic acid, copper sulfate and uric acid; and recording by adopting a current-time method, and observing the change condition of adding different interference currents. The selectivity of NiO/PDDA-RGO/GCE was examined. It can be seen from fig. 5 that the current is significantly increased after the addition of sodium nitrite, and the change caused by the addition of interferent compared to the addition of sodium nitrite is negligible. Therefore, the sensor has good selectivity and interference resistance.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the concept and the protection scope of the present invention, and those skilled in the art should make various modifications and improvements to the technical solution of the present invention without departing from the design concept of the present invention.
Claims (9)
1. A preparation method of a three-dimensional flower-like nano composite NiO/PDDA-RGO is characterized by comprising the following steps:
1) preparation of PDDA-RGO:
dissolving 15-50mg of graphene oxide in 15-25mL of deionized water, carrying out ultrasonic treatment for 0.5-3h to obtain a graphene oxide dispersion solution, and then placing the graphene oxide dispersion solution in a container; then, taking 5-10.0 mL of graphene oxide dispersion liquid with the concentration of 1.0-2.0 mg/mL into a reaction bottle, adding 50.0-60.0 mu L of PDDA with the concentration of 8.0-12.0 wt%, fully stirring and uniformly mixing, and then adjusting the pH value to 9-10.0 by using concentrated ammonia water; adding 40.0-55.0 mu L of 80% hydrazine hydrate, stirring vigorously, placing the reaction bottle in a 50-80 ℃ water bath kettle, heating for 3-4h, cooling to room temperature, washing and drying the synthesized material to obtain PDDA-RGO;
2) preparing three-dimensional flower-like NiO:
adding 0.06-0.07g NH4F，0.2-0.3g Ni(NO3)2.6H2Adding 0.3-0.5g of urea into a mixed solution of 20mL of distilled water and 0.635mL of glycol in sequence, uniformly stirring the solution for 0.5-1h, transferring the solution into a 50mL reaction kettle, and reacting at the temperature of 130 ℃ for 8-10 h; centrifugally washing the light blue liquid obtained after the reaction is finished, and drying the liquid for 2 hours at the temperature of 80 ℃ to obtain light blue powder; placing the crucible containing the powder in a muffle furnace at 5 deg.C for min-1Heating at 380-400 ℃ for reaction for 2-3h to obtain three-dimensional flower-shaped NiO;
3) preparing a three-dimensional flower-like nano composite NiO/PDDA-RGO:
firstly, 10-30mg of PDDA-RGO synthesized in the step 1) is subjected to ultrasonic treatment in 10-30mL of distilled water for 0.5-1h, 1.25-20mg of three-dimensional flower-shaped NiO synthesized in the step 2) is added after the PDDA-RGO is completely and uniformly dispersed, and ultrasonic treatment is carried out for 2-3h at room temperature, so as to obtain the three-dimensional flower-shaped nano composite NiO/PDDA-RGO.
2. The method for preparing NiO/PDDA-RGO according to claim 1, wherein the graphene oxide ultrasonic treatment time in step 1) is 3h, the graphene oxide dispersion concentration is 1mg/mL, and the PDDA concentration is 10.0 wt%.
3. The method for preparing NiO/PDDA-RGO according to claim 1, wherein the heating temperature of the water bath in step 1) is 60 ℃ and the heating time is 4 h.
4. The method for preparing NiO/PDDA-RGO according to claim 1, wherein the mixed solution in the step 2) is stirred for 1h, and the reaction is carried out in the reaction kettle at 130 ℃ for 10 h; the light blue powder was calcined in a muffle furnace at 400 ℃ for 3 h.
5. The method for preparing NiO/PDDA-RGO according to claim 1, wherein the ultrasonic treatment time after mixing in step 3) is 3 h.
6. NiO/PDDA-RGO prepared by the method of any one of claims 1 to 5.
7. Use of the NiO/PDDA-RGO of claim 6 in nitrite detection.
The preparation method of the NiO/PDDA-RGO modified electrode is characterized by comprising the following steps: polishing the surface of the naked GCE with 0.05 μm of alumina particles, carefully washing with ultrapure water and ethanol until a mirror surface is obtained and drying, removing 6-8 μ L of NiO/PDDA-RGO of claim 6 to be dripped on the surface of a Glassy Carbon Electrode (GCE), and fully baking under an infrared lamp to obtain the NiO/PDDA-RGO modified electrode (NiO/PDDA-RGO/GCE).
9. A method of detecting nitrite, comprising the steps of: preparing a series of sodium nitrite standard solutions with different concentrations, using the NiO/PDDA-RGO modified electrode prepared according to claim 8 as a working electrode, a platinum wire electrode as a counter electrode, a silver-silver chloride electrode as a reference electrode, placing the three electrodes in a solution using 0.1M phosphate buffer solution (pH 5) as an electrolyte, recording peak currents corresponding to sodium nitrite with different concentrations by adopting a current-time method, and drawing a standard curve of current versus concentration according to the peak current value and the concentration of sodium nitrite in the corresponding standard solution.
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| CN111974409A (en) * | 2020-08-13 | 2020-11-24 | 扬州大学 | Flaky porous manganese-doped nickel oxide catalyst, preparation method and application thereof |
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| CN112010359A (en) * | 2020-07-09 | 2020-12-01 | 江苏大学 | NiO/C nano composite electrode material and preparation method and application thereof |
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| CN113120976A (en) * | 2021-04-21 | 2021-07-16 | 吉林大学 | Ni4OHF7 electrode material and preparation method and application thereof |
| CN113120976B (en) * | 2021-04-21 | 2021-12-10 | 吉林大学 | Ni4OHF7 electrode material and preparation method and application thereof |
| CN113791121A (en) * | 2021-09-30 | 2021-12-14 | 杭州汇馨传感技术有限公司 | Ternary composite gas sensing chip, preparation method and application method thereof, and gas sensing material |
| CN114188163A (en) * | 2021-12-08 | 2022-03-15 | 吉林大学 | NiO wool spherical electrode material and preparation method and application thereof |
| CN114188163B (en) * | 2021-12-08 | 2023-01-24 | 吉林大学 | NiO wool spherical electrode material and preparation method and application thereof |
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Application publication date: 20200414 |