Molybdenum sulfide multi-walled carbon nanotube gold modified glassy carbon electrode

A technology of multi-walled carbon nanotubes and glassy carbon electrodes, which is applied in the direction of material electrochemical variables, can solve problems such as poisoning and canceration, and achieve the effects of simple structure, high sensitivity, and improved electrocatalytic performance

Inactive Publication Date: 2017-05-31
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Studies have shown that nitrite can be converted into nitrosamines under cer

Method used

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  • Molybdenum sulfide multi-walled carbon nanotube gold modified glassy carbon electrode
  • Molybdenum sulfide multi-walled carbon nanotube gold modified glassy carbon electrode
  • Molybdenum sulfide multi-walled carbon nanotube gold modified glassy carbon electrode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Weigh 1.0 mmol of sodium molybdate dihydrate and 4 mmol of thiourea in deionized water to form a mixed solution (1);

[0043] (2) Weigh 0.4 g of multi-walled carbon nanotubes, add them into the mixed solution (1), stir evenly, and form the mixed solution (2);

[0044] (3) Transfer the mixed solution (2) to a high-pressure reactor and react at 200 °C;

[0045] (4) After the reaction product of step (3) is centrifuged to remove moisture, first wash with ethanol to remove organics such as unreacted thiourea, and then wash with deionized water to remove unreacted inorganic ions until the pH value of the solution is 7.0, and the cleaned The final reaction product is placed in an oven and dried at 65°C to obtain a molybdenum sulfide multi-walled carbon nanotube composite;

[0046] figure 1 Scanning electron micrograph of the molybdenum sulfide multi-walled carbon nanotube composite prepared for the present invention.

Embodiment 2

[0048] a) Weigh 4 mg of the molybdenum sulfide multi-walled carbon nanotube composite of Example 1 and add 80 microliters of perfluorosulfonic acid to a mixture of 0.25 microliters of deionized water and 0.75 milliliters of ethanol, and mix well by ultrasonic;

[0049] b) Apply an appropriate amount of 5 microliters of the homogeneous mixed solution obtained in step a) onto the surface of a clean glassy carbon electrode, and dry at room temperature;

[0050] c) the glassy carbon electrode obtained in step b), a platinum wire and a saturated calomel electrode are used to form a three-electrode system;

[0051] d) Put the three-electrode system into a sulfuric acid solution containing 3 mmol / L of chloroauric acid, electrolyze at -0.4 volts, after 20 seconds of electrolysis, remove the working electrode, and wash with deionized water to obtain Molybdenum sulfide multi-walled carbon nanotube gold nanocomposite modified glassy carbon electrode.

[0052] The morphology and material...

Embodiment 3

[0054] ① A three-electrode system composed of molybdenum sulfide multi-walled carbon nanotube gold nanocomposite modified glassy carbon electrode, platinum wire and saturated calomel electrode was placed in phosphate buffer solution containing different concentrations of nitrite, and determined by differential pulse voltammetry The catalytic performance of molybdenum sulfide multi-walled carbon nanotube gold nanocomposite to nitrite, the potential range of differential pulse voltammetry is 0~1.5 volts;

[0055]② Put the three-electrode system in step ① into a phosphate buffer solution with a constant concentration, add sodium nitrite solutions of different concentrations dropwise, measure the corresponding response current values ​​of sodium nitrite solutions with different concentrations by constant potential method, and prepare The linear relationship graph between the concentration of nitrite and the response current was obtained, and the potential range of the constant pote...

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Abstract

The invention discloses a molybdenum sulfide multi-walled carbon nanotube gold modified glassy carbon electrode. A preparation method comprises the following steps of dispersing a multi-walled carbon nanotube into a solution of thiourea and a sodium molybdate dihydrate, uniformly agitating an obtained first mixture, and then transferring the first mixture into a high-pressure reaction kettle to carry out a reaction; centrifugally separating an obtained reaction product, and then washing the reaction product by using ethyl alcohol and deionized water; oven-drying the reaction product to obtain a molybdenum sulfide multi-walled carbon nanotube finished product; taking and dispersing a molybdenum sulfide multi-walled carbon nanotube compound in mixed liquor of water, ethyl alcohol and perfluorosulfonic acid, and dropwise coating the clean surface of a glassy carbon electrode with an obtained second mixture; naturally air-drying the glassy carbon electrode, and then using the glassy carbon electrode as a working electrode to form a three-electrode system with a platinum wire and a saturated calomel electrode; putting the three-electrode system in a sulfuric acid solution containing chloroauric acid, and carrying out constant-potential electrolysis, so as to obtain a molybdenum sulfide multi-walled carbon nanotube gold nano compound modified glassy carbon electrode. Proven by a result, a molybdenum sulfide multi-walled carbon nanotube gold nano compound can be used for the effective catalytic oxidation of nitrite, is used for detecting the nitrite conveniently and quickly, is high in sensitivity and is wide in concentration detection range.

Description

technical field [0001] The invention relates to the field of composite material preparation, in particular to a molybdenum sulfide multi-walled carbon nanotube gold-modified glassy carbon electrode. Background technique [0002] Micropollutants in water, such as nitrite, bromate, perchlorate, etc., are potentially harmful to the health of humans and aquatic animals and plants. Among these micropollutants, nitrite is commonly used in fertilizers and the food processing industry, and can be transferred to water or the human body through food. Studies have shown that nitrite can be converted into nitrosamines under certain conditions, which can cause serious toxic effects and even cause cancer. Therefore, real-time detection of nitrite in water is very important. There are many methods for detecting nitrite, such as ion chromatography, electrochemical method, etc. Among them, the electrochemical method is simple to operate, high in sensitivity, and good in portability, and is...

Claims

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Application Information

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IPC IPC(8): G01N27/30
CPCG01N27/30
Inventor 张娅谈晶温芳芳周芝峰王宏归张子岚
Owner YANGZHOU UNIV
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