CN110646482A - Three-dimensional nano spherical polyaniline/MnO2+Mn3O4Preparation of non-enzyme ascorbic acid electrochemical sensor - Google Patents
Three-dimensional nano spherical polyaniline/MnO2+Mn3O4Preparation of non-enzyme ascorbic acid electrochemical sensor Download PDFInfo
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Abstract
The invention belongs to the technical field of nano functional materials and electrochemistry, and particularly relates to three-dimensional nano spherical polyaniline/MnO2+Mn3O4A preparation method of a non-enzymatic ascorbic acid electrochemical sensor. The invention firstly prepares MnOx by a simple chemical method, and then adds the MnOx into aniline solution to carry out in-situ polymerization to synthesize PANI/MnO2+Mn3O4Composite material, PANI/MnO prepared by modifying it on glassy carbon electrode2+Mn3O4Non-enzymatic sensors and will be used for ascorbic acid detection. The result shows that the three-dimensional nano spherical PANI/MnO prepared by the invention2+Mn3O4The non-enzymatic ascorbic acid electrochemical sensor has the advantages of simple preparation, good reproducibility and repeatability, high stability, strong anti-interference capability and the like, and has great development prospect in the industries of food monitoring, medical care and the like.
Description
Technical Field
The invention belongs to the technical field of nano functional materials and electrochemistry, and particularly relates to three-dimensional nano spherical polyaniline-MnO2+Mn3O4(PANI/MnO2+Mn3O4) And (3) preparing a non-enzymatic ascorbic acid electrochemical sensor.
Background
An electrochemical sensor is a sensor that converts a chemical signal of a substance to be detected into an electric signal based on the electrochemical properties of the substance to be detected, and then analyzes the electric signal. Electrochemical sensors are classified into various types, and the sensors may be classified into electrochemical sensors and non-enzymatic electrochemical sensors according to bioactive materials modified on electrodes. The material of the non-enzyme sensor modified electrode has biological catalytic activity, such as metal and oxide nanometer materials thereof, carbon materials and conductive high polymer materials.
Ascorbic Acid (AA), also commonly referred to as vitamin C, is readily soluble in water and has some reducibility. Ascorbic acid is important for the normal functioning of metabolic processes in the human body, and the absence of ascorbic acid leads to the development of scurvy. In addition, ascorbic acid is widely used in the food, cosmetic and other industries because of its antioxidant properties. The ascorbic acid is usually measured by spectrophotometry, fluorescence, high performance liquid chromatography, chemical titration, electrochemical analysis, and the like. These methods have advantages, but have disadvantages and limitations, or they have low detection sensitivity, large error in the result, expensive equipment, complicated analysis steps and methods, and the like, which limit their application to ascorbic acid detection. Along with the development and utilization of novel sensors, the electrochemical sensor is utilized to detect the ascorbic acid, so that the method is low in cost, convenient and fast, high in sensitivity, good in selectivity and strong in anti-interference capability, and has great advantages and practical value.
Polyaniline (PANI) is a common conductive polymer, and can be used for preparing various devices and materials with special functions and meeting specific requirements after being doped with protonic acid, such as modified electrode materials of sensors, lithium battery materials, electron field emission sources and the like. The polyaniline is used as a modified electrode, so that the influence of electrolyte on the electrode can be effectively reduced, substances on the surface of the electrode are prevented from entering the electrolyte, the pollution to the electrolyte is reduced, and the detection sensitivity is improved. And secondly, the polyaniline has higher electrical activity and can be used as an intermediate for electron transfer in oxidation-reduction reaction and enzymatic reaction, so that the electron transfer is greatly accelerated, an electric signal is amplified, and the detection sensitivity is improved. In addition, the polyaniline has the advantages of easily obtained raw materials, simple and convenient synthesis method, high stability and unique use advantage as a sensor electrode material, and can be synthesized in a liquid phase.
Metal oxides are a functional inorganic material widely used in daily life. The metal oxide is very expensive and can constitute a large number of crystal structures having various morphologies and having different electronic structures, so that the oxide can exhibit characteristics of a metal, a semiconductor, or an insulator. These different crystal structures cause the metal oxide material to have different crystal plane activities and specific surface areas, thereby affecting the physical and chemical properties of the metal oxide material. Metal oxides are often used as electrode materials because they have a porous structure, large pore diameters, and a high specific surface area, and can undergo a relatively complete redox reaction. At present, metal oxide materials with rich and various properties are widely applied to the fields of photocatalysis, sensor materials, plasma batteries and the like.
Disclosure of Invention
Based on the reasons, the invention provides three-dimensional nano spherical PANI/MnO2+Mn3O4And (3) preparing a non-enzymatic ascorbic acid electrochemical sensor. The invention relates to three-dimensional nano spherical PANI/MnO2+Mn3O4The preparation method of the non-enzymatic ascorbic acid electrochemical sensor comprises the following specific steps:
(1) weighing a certain amount of KMnO4And MnSO4·H2Placing the O sample in a 100 mL beaker, adding deionized water at room temperature to prepare a uniform and transparent solution, and continuously stirring for a plurality of hours by using a magnetic stirrer, wherein the maximumA black precipitate was obtained. Washing with deionized water and anhydrous ethanol for three times, drying in 70 deg.C oven, and grinding to obtain MnO2+Mn3O4And (3) powder.
(2) Weighing aniline and sodium dodecyl benzene sulfonate in a certain proportion, placing the aniline and the sodium dodecyl benzene sulfonate into a 100 mL beaker, and simultaneously adding a proper amount of MnO prepared in the step (1)2+Mn3O4And adding a certain amount of protonic acid for dissolution, and marking as solution A. Then 1.5 g of ammonium persulfate was weighed and dissolved in the same volume of the same concentration of the protonic acid, and the solution was recorded as solution B. Slowly dripping solution B (about 3 s per drop, 0 deg.C, stirring) into solution A, stirring in ice water bath for 8 hr, filtering, washing to obtain dark green product, oven drying at 60 deg.C, and grinding to obtain dark green homogeneous powder PANI/MnO2+Mn3O4A composite material.
(3) Weighing a certain amount of prepared PANI/MnO2+Mn3O4Dissolving the powder in a certain amount of deionized water to prepare a solution, and performing ultrasonic treatment to uniformly mix the solution and the solution to obtain the required dispersion liquid. Measuring 5 mu L PANI/MnO with a pipette2+Mn3O43Uniformly dripping the dispersion liquid to the center of a glassy carbon electrode, and drying under an ultraviolet lamp to obtain PANI/MnO2+Mn3O4Modified electrode, i.e. PANI/MnO2+Mn3O4A non-enzymatic sensor.
Further, step (1) KMnO4And MnSO4·H2The molar ratio of O is 0.1:0.15, the continuous stirring time of a magnetic stirrer is 6 ~ 8h, and the drying in an oven at 70 ℃ is 10 ~ 12 h.
Further, in the step (2), the ratio of aniline to sodium dodecylbenzenesulfonate is 1: 0.25, and the amount of ethanol added is 150 ~ 200 mL.
Further, the protonic acid in step (2) may be H2SO4HCl, p-toluenesulfonic acid and protonic acid, wherein the addition amount of the protonic acid is 40 ~ 60 mL, and the concentration is 0.5 ~ 1.0.0 mol/L.
Further, MnO in step (2)2+Mn3O4Is added in an amount ofThe mass ratio of the added aniline is 1 ~ 5:1 ~ 5.
Further, in the step (2), stirring is carried out for 8 ~ 10 hours under the condition of ice-water bath at the temperature of 0 ℃, and drying time in an oven at the temperature of 60 ℃ is 6 ~ 8 hours.
Further, PANI/MnO in step (3)2+Mn3O4The powder was weighed as 2 ~ 6 mg, dissolved in 2 ~ 6 mL deionized water and dispersed ultrasonically for 30 ~ 60 minutes, and dried under infrared lamp for 20 ~ 50 minutes.
The invention has the beneficial effects that:
three-dimensional nano spherical PANI/MnO prepared by the invention2+Mn3O4The non-enzymatic ascorbic acid electrochemical sensor has the advantages of simple preparation, good reproducibility and repeatability, high stability, strong anti-interference capability and the like, and has great development prospect in the industries of food monitoring, medical care and the like.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is the three-dimensional nano-spherical PANI/MnO in example 12+Mn3O4Non-enzymatic ascorbic acid electrochemical sensor XRD patterns.
FIG. 2 is the three-dimensional nano-spherical PANI/MnO in example 12+Mn3O4SEM image of non-enzyme ascorbic acid electrochemical sensor.
FIG. 3 shows the three-dimensional nano-spherical PANI/MnO in comparative example 12+Mn3O4And comparing the electrochemical performances of the non-enzyme ascorbic acid electrochemical sensor.
Detailed Description
The invention will now be further illustrated by reference to specific examples, which are intended to be illustrative of the invention and are not intended to be a further limitation of the invention.
Example 1:
PANI/MnO2+Mn3O4the non-enzymatic ascorbic acid electrochemical sensor comprises the following steps:
（1）1.58 g KMnO4and 2.535 g MnSO4•H2The O sample was placed in a 100 mL beaker and 1 was added00 mL of distilled water is prepared into 0.10 mol/L KMnO4Solution and 0.15 mol/L MnSO4And mixing the solution and the solution at room temperature, and continuously stirring for 6 hours by using a magnetic stirrer to finally obtain black precipitate. Washing with deionized water and anhydrous ethanol for three times, drying in 70 deg.C oven for 12 hr, and grinding to obtain MnO2+Mn3O4And (3) powder.
(2) Weighing 1.0 g of aniline and 0.25 g of sodium dodecyl benzene sulfonate, placing the aniline and the sodium dodecyl benzene sulfonate into a 100 mL beaker, and simultaneously adding 0.2 g of MnO prepared in the step (1)2+Mn3O4Powder, adding 40 mL0.5 mol/L H2SO4Dissolve and mix well to obtain solution A. Then 1.5 g of ammonium persulfate was weighed and dissolved in 20 mL of 0.5 mol/L H2SO4In (1), denoted as solution B. Slowly dropwise adding the solution B into the solution A (about 3 seconds per drop, 0 ℃, stirring), continuously stirring for 8 hours under the condition of ice-water bath, filtering and washing to obtain a dark green product, drying in an oven at 60 ℃, and grinding to obtain dark green homogeneous powder.
(3) Weighing 4 mg of uniformly ground polyaniline-metal oxide powder, placing the powder into a 2 mL sample tube, dissolving the powder with deionized water to prepare the polyaniline-metal oxide powder with the concentration of 2 mg ∙ mL-1The dispersion liquid of (2) is placed in an ultrasonic cleaner for 30 minutes to be uniformly dispersed. And finally, accurately sucking 10 muL of dispersion liquid by using a micropipettor, and dripping the dispersion liquid on the glassy carbon electrode to enable the solution to be uniformly attached to the surface of the electrode. Dropwise adding 5 mu L Nafion solution after solidification and film formation, and drying under an infrared lamp to obtain PANI/MnO2+Mn3O4An electrochemical non-enzymatic sensor.
FIG. 1 is a three-dimensional nano spherical PANI/MnO prepared2+Mn3O4XRD pattern of non-enzyme ascorbic acid electrochemical sensor, in figure 2θThere are two stronger peaks at = 21 ° and 25 °, corresponding to (020) and (200) of PANI. For PANI/MnO2+Mn3O4At 2θThe diffraction peak appearing at = 28.851 ° corresponds to the (110) crystal face of JCPDS NO.50-0866 of manganese dioxide PDF standard card, except that in 2θ= 36.040 degree of appearance of trimanganese tetroxide PDF standard card JCPDS No.18-08031) Crystal face, demonstrates PANI/MnO2+Mn3O4Successful synthesis of the compound; FIG. 2 is an SEM image of a three-dimensional nano spherical PANI/MnO2+ Mn3O4 non-enzymatic ascorbic acid electrochemical sensor, in which three-dimensional nano spheres with the diameter of hundreds of nanometers are uniformly dispersed and clearly visible, and further proves that the three-dimensional nano spherical PANI/MnO are2+Mn3O4The non-enzymatic ascorbic acid electrochemical sensor was successfully prepared.
Example 2:
mixing PANI/MnO2+Mn3O4Placing the non-enzymatic ascorbic acid electrochemical sensor in PBS buffer solution containing 0.20 mmol/L ascorbic acid, pH = 7.0 and 0.20 mol/L, forming a three-electrode system with a Pt sheet electrode and a calomel electrode, setting the scanning speed to be 100 mV/s, and arranging aniline and MnO2The mass ratio of (A) to (B) is 5:1, cyclic voltammetry curve measurement is performed.
Comparative example 1:
the metal oxide in step (1) of example 1 was changed to CeO2Controlling the rest conditions unchanged, aniline and CeO2The mass ratio of (A) to (B) is 5:1 to synthesize the PANI/CeO2(5:1) non-enzymatic electrochemical sensor. The ascorbic acid response effect in the phosphate buffer solution of PBS was measured by the same measurement method as in example 2. The test result shows that PANI/MnO2+Mn3O4The non-enzymatic electrochemical performance is obviously superior to PANI/CeO2(FIG. 3). Illustrates the three-dimensional nano spherical PANI/MnO prepared by the invention2+Mn3O4Non-enzymatic ascorbic acid electrochemical sensor is compared with PANI/CeO in ascorbic acid detection2Has stronger electrochemical activity.
Claims (7)
1. Three-dimensional nano spherical PANI/MnO2+Mn3O4The preparation of non-enzyme ascorbic acid electrochemical sensor is characterized by comprising the following main steps:
(1) weighing a certain amount of KMnO4And MnSO4·H2Placing the O sample in a 100 mL beaker, adding deionized water at room temperature to prepare a uniform and transparent solution, and adopting a magnetic stirrerContinuously stirring for several hours to obtain black precipitate, washing with deionized water and anhydrous ethanol for three times, drying in 70 deg.C oven, and grinding to obtain MnO2+Mn3O4Powder;
(2) weighing aniline and sodium dodecyl benzene sulfonate in a certain proportion, placing the aniline and the sodium dodecyl benzene sulfonate into a 100 mL beaker, and simultaneously adding a proper amount of MnO prepared in the step (1)2+Mn3O4Adding a certain amount of protonic acid for dissolving, marking as solution A, weighing 1.5 g of ammonium persulfate to dissolve in the protonic acid with the same volume and concentration, marking as solution B, slowly dropwise adding the solution B into the solution A (about 3 seconds per drop, 0 ℃, stirring), then continuously stirring for 8 hours under the condition of ice-water bath, filtering and washing to obtain a dark green product, drying in an oven at 60 ℃, and grinding to obtain dark green homogeneous powder PANI/MnO2+Mn3O4A composite material;
(3) weighing a certain amount of prepared PANI/MnO2+Mn3O4Dissolving the powder in a certain amount of deionized water to obtain a solution, mixing with ultrasonic wave to obtain a desired dispersion, and measuring 5 μ L PANI/MnO with a pipette2+Mn3O43Uniformly dripping the dispersion liquid to the center of a glassy carbon electrode, and drying under an ultraviolet lamp to obtain PANI/MnO2+Mn3O4Modified electrode, i.e. PANI/MnO2+Mn3O4A non-enzymatic sensor.
2. The three-dimensional nano-spherical PANI/MnO of claim 12+Mn3O4The preparation method of the non-enzyme ascorbic acid electrochemical sensor is characterized by comprising the following steps: step (1) KMnO4And MnSO4·H2The molar ratio of O is 0.1:0.15, the continuous stirring time of a magnetic stirrer is 6 ~ 8h, and the drying in an oven at 70 ℃ is 10 ~ 12 h.
3. The three-dimensional nano-spherical PANI/MnO of claim 12+Mn3O4Preparation method of non-enzymatic ascorbic acid electrochemical sensorThe method is characterized in that in the step (2), the ratio of aniline to sodium dodecyl benzene sulfonate is 1: 0.25, and the adding amount of ethanol is 150 ~ 200 mL.
4. The three-dimensional nano-spherical PANI/MnO of claim 12+Mn3O4The preparation method of the non-enzyme ascorbic acid electrochemical sensor is characterized by comprising the following steps: the protonic acid in the step (2) may be H2SO4HCl, p-toluenesulfonic acid and protonic acid, wherein the addition amount of the protonic acid is 40 ~ 60 mL, and the concentration is 0.5 ~ 1.0.0 mol/L.
5. The three-dimensional nano-spherical PANI/MnO of claim 12+Mn3O4The preparation method of the non-enzyme ascorbic acid electrochemical sensor is characterized by comprising the following steps: MnO in step (2)2+Mn3O4The mass ratio of the addition amount of (2) to the addition amount of aniline is 1 ~ 5:1 ~ 5.
6. The three-dimensional nano-spherical PANI/MnO of claim 12+Mn3O4The preparation method of the non-enzymatic ascorbic acid electrochemical sensor is characterized in that in the step (2), the mixture is stirred for 8 ~ 10 hours under the condition of ice-water bath at 0 ℃, and the drying time in an oven at 60 ℃ is 6 ~ 8 hours.
7. The three-dimensional nano-spherical PANI/MnO of claim 12+Mn3O4The preparation method of the non-enzyme ascorbic acid electrochemical sensor is characterized by comprising the following steps: in step (3), PANI/MnO2+Mn3O4The powder was weighed as 2 ~ 6 mg, dissolved in 2 ~ 6 mL deionized water and dispersed ultrasonically for 30 ~ 60 minutes, and dried under infrared lamp for 20 ~ 50 minutes.
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| CN111426644A (en) * | 2020-03-18 | 2020-07-17 | 广东工业大学 | IrO (IrO)2/MnO2Composite nano enzyme and preparation method and application thereof |
| CN111595920A (en) * | 2020-05-26 | 2020-08-28 | 济南大学 | Electrochemical detection method for imidacloprid by loading polyaniline on surface of biomass-derived porous carbon |
| CN112240901A (en) * | 2020-10-21 | 2021-01-19 | 南京工业大学 | Simple preparation method of glycerol biosensor chip |
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| CN112240901A (en) * | 2020-10-21 | 2021-01-19 | 南京工业大学 | Simple preparation method of glycerol biosensor chip |
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Application publication date: 20200103 |