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Preparation method and application of rod-like nickel disulfide-molybdenum disulfide nano-composite

A nanocomposite, nickel disulfide technology, applied in the direction of nickel sulfide, molybdenum sulfide, material electrochemical variables, etc., can solve the problems of small specific surface area, low activity of nickel disulfide, etc., to achieve simple synthesis, low cost, excellent subsurface The effect of nitrate on the properties

Active Publication Date: 2020-07-17
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, common monomer nickel disulfide has low activity and small specific surface area

Method used

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  • Preparation method and application of rod-like nickel disulfide-molybdenum disulfide nano-composite
  • Preparation method and application of rod-like nickel disulfide-molybdenum disulfide nano-composite
  • Preparation method and application of rod-like nickel disulfide-molybdenum disulfide nano-composite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1), respectively weigh 1.5 grams of nickel nitrate hexahydrate and 1.5 grams of sodium thiosulfate pentahydrate in deionized water, and stir for 5 minutes;

[0048] (2), take by weighing 30mg cetyl trimethyl ammonium bromide and add in the mixed solution obtained in step (1) and stir for 10 minutes;

[0049] (3) Add 8ml of ethylenediamine to the mixed solution obtained in step (2), stir evenly, transfer it to a high-pressure reaction kettle, and react at 160°C for 20h;

[0050] (4) After centrifuging the reaction product in step (3) to remove water, first wash with ethanol to remove unreacted organic matter, then wash with deionized water to remove unreacted inorganic ions, and place the washed reaction product in a Dry in an oven at 70°C;

[0051] (5), placing the product obtained in step (4) in a tube furnace, passing argon gas, and calcining at 300 ° C for 2 hours to obtain nickel disulfide;

[0052] (6), respectively weigh 130mg ammonium tetrathiomolybdate and 60...

Embodiment 2

[0061] The three-electrode system prepared in Example 1 was placed in a solution containing no and 1, 2, and 4 mmol dm -3 0.1mol dm of sodium nitrite -3 The catalytic performance of rod-shaped nickel disulfide-molybdenum disulfide complexes for nitrite was determined by cyclic voltammetry in phosphate buffer solution. The cyclic voltammogram is shown in figure 2 shown.

[0062] figure 2 Modified glassy carbon electrodes for rod-shaped nickel disulfide-molybdenum disulfide composites without and with 1, 2, and 4 mmoldm -3 0.1 mol dm of sodium nitrite -3 Cyclic voltammogram in phosphate buffered solution. It can be seen from the figure that when the composite modified glassy carbon electrode was moved from the phosphate buffer solution to the solution containing sodium nitrite, an oxidation peak appeared near 0.3 V, and the peak appeared with the increase of nitrite concentration. the current increases. This result indicates that nitrite undergoes a reduction reaction at...

Embodiment 3

[0065] The three-electrode system prepared in Example 1 was placed in 0.1 mol dm -3 In the phosphate buffer solution, sodium nitrite solutions of different concentrations were added dropwise, and the response current values ​​corresponding to different concentrations of sodium nitrite solutions were measured by potentiostatic method, and the linear relationship between the concentration of nitrite and the response current was obtained ( image 3 );

[0066] from image 3 It can be seen from: rod-shaped nickel disulfide-molybdenum disulfide composite modified glassy carbon electrode for 0.1 mmol dm -3 nitrite can respond. Figure 4 is true image 3 A plot of nitrite concentration versus response current. As can be seen from the graph: at 8 to 4300µmol dm -3 A good linear relationship is maintained within the range of .

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Abstract

The invention relates to a preparation method and application of a rod-like nickel disulfide-molybdenum disulfide nano composite. The preparation method comprises the following steps: dispersing nickel nitrate hexahydrate and sodium thiosulfate pentahydrate in deionized water, adding hexadecyl trimethyl ammonium bromide, stirring, adding ethylenediamine, uniformly stirring, transferring into a high-pressure reaction kettle for reaction, centrifugally separating, cleaning with ethanol and deionized water, drying, calcining in a tubular furnace to obtain nickel disulfide, weighing ammonium tetrathiomolybdate and nickel disulfide, adding ammonium tetrathiomolybdate and nickel disulfide into an N,N-dimethylformamide solution, adding hydrazine hydrate, carrying out ultrasonic treatment, transferring the mixed solution into a high-pressure reaction kettle for reaction, centrifugally separating, cleaning with ethanol and deionized water, drying to obtain a rod-like nickel disulfide-molybdenumdisulfide nano-composite, dispersing the composite into a mixed solution of water, ethanol and perfluorosulfonic acid, dropwise coating on the surface of a clean glassy carbon electrode and naturallyair-drying to form a three-electrode system together with a platinum wire and a saturated calomel electrode, wherein the clean glassy carbon electrode is used as a working electrode.

Description

technical field [0001] The invention relates to a preparation method and application of a rod-shaped nickel disulfide-molybdenum disulfide nanocomposite, belonging to the technical field of environmental detection. Background technique [0002] At present, nitrite pollution in water resources has received special attention. In many countries, drinking water extracted from groundwater is increasingly polluted by nitrite and nitrate, endangering public health. It will cause human health problems, Such as kidney damage and blue baby syndrome, or become the precursor of carcinogens, leading to cancer; therefore, the real-time detection of nitrite is a very necessary and meaningful thing. Electrochemical method is one of the commonly used methods to detect nitrite, and it is an environmentally friendly technology. Compared with fluorescence spectrophotometry, chemiluminescence and chromatography, electrochemical sensing technology has high sensitivity, fast response, and easy min...

Claims

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Application Information

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IPC IPC(8): C01G53/11C01G39/06G01N27/30G01N27/416G01N27/48
CPCC01G53/11C01G39/06G01N27/308G01N27/4166G01N27/48C01P2006/40C01P2004/03C01P2004/16Y02E60/10
Inventor 王宏归潘华伟张娅
Owner YANGZHOU UNIV
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