Flower wall-shaped Mn-Fe prussian blue analogue material and preparation method and application thereof
A Prussian blue and flower-shaped technology, applied in the field of electrochemical detection, can solve the problem of high detection limit of chemically modified electrodes, and achieve the effects of improved detection limit and sensitivity, good stability, and strong anti-interference
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[0037] Example 1 Preparation of spherical Mn-Fe Prussian blue analog material
[0038] (1) Weigh 0.165g K 3 [Fe(CN) 6 ] In a beaker, add 20 mL of deionized water to dissolve it to obtain liquid A;
[0039] (2) Weigh out 0.063g MnCl 2 Place it in another beaker and add 20mL of deionized water to dissolve it to obtain liquid B;
[0040] (3) Transfer liquid B to a round-bottomed flask, slowly add liquid A under the condition of magnetic stirring, the mixed liquid was reacted with magnetic stirring for 24h, then centrifuged, washed and dried with deionized water to obtain a spherical Mn-Fe Prussian Blue analog material.
[0041] The morphology, structure and composition characteristics of the spheroidal Mn-Fe Prussian blue analog material prepared in this example are as follows: figure 1 It is the scanning electron micrograph (A), X-ray powder diffraction pattern (B), infrared spectrum (C) and photoelectron spectrum (D) of the spheroidal Mn-Fe Prussian blue analog material. From figure 1 A.
Example Embodiment
[0055] Example 2 Preparation of spheroidal Mn-Fe Prussian blue analog material modified electrode
[0056] (1) Take a glassy carbon electrode with a diameter of 3mm, wash the glassy carbon electrode with water, and then there is an appropriate amount of Al with a particle size of 0.05μm. 2 O 3 The powder is polished with a figure of eight, polished 50 times and then washed with deionized water, then washed with dilute nitric acid, acetone and deionized water ultrasonically, and dried under infrared light to obtain pretreated glassy carbon electrode;
[0057] (2) Take 3 mg of the curdled Mn-Fe Prussian blue analog material described in Example 1 and disperse it in 5 mL of N,N-dimethylformamide solvent for 10 minutes to obtain an electrode material modification solution;
[0058] (3) Take 4μL of electrode material dispersion and apply it to the surface of the pretreated glassy carbon electrode, and then dry it to obtain a spheroidal Mn-Fe Prussian blue analog material modified electrode.
Example Embodiment
[0060] Example 3 The detection performance of the spheroidal Mn-Fe Prussian blue analog material modified electrode
[0061] In this example, the modified electrodes prepared in Example 2 were used as the experimental objects, and the platinum sheet auxiliary electrode and the saturated calomel reference electrode constituted a three-electrode system, and connected to the CHI660 electrochemical workstation (Shanghai Chenhua Instrument Co., Ltd.). Electrochemical performance testing.
[0062] (1) Comparison of electrocatalytic reduction performance of 2,4-dinitrophenol with different electrodes
[0063] In order to more intuitively reflect the electrocatalytic reduction performance of the curdled Mn-Fe Prussian blue analogue material modified electrode prepared by the present invention to 2,4-dinitrophenol, the curdled Mn-Fe Prussian blue analogue material was modified The electrodes were placed in a blank base solution (a) and a base solution containing 80μmol / L 2,4-dinitrophenol (b)
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