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Nano nickel-sulfur compound based on eutectic solvent one-step synthesis method

A technology of deep eutectic solvent and sulfur compound is applied in the field of preparing nano-nickel sulfur compound by one-step synthesis method of deep eutectic solvent, which can solve the problems of expensive equipment, high impurity content and high reaction temperature, and achieves low price, high purity, The effect of low temperature requirements

Active Publication Date: 2019-08-30
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the methods for preparing nickel-sulfur compounds mainly include high-temperature solid-phase method, high-energy ball milling method, hydrothermal / solvothermal method, spray pyrolysis / drying method, etc., but these methods generally have high equipment requirements, high reaction temperature, and long preparation time. , expensive equipment, many processes, complicated operation, high impurity content, etc.

Method used

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  • Nano nickel-sulfur compound based on eutectic solvent one-step synthesis method
  • Nano nickel-sulfur compound based on eutectic solvent one-step synthesis method
  • Nano nickel-sulfur compound based on eutectic solvent one-step synthesis method

Examples

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Effect test

example 1

[0048] Deep eutectic solvent one-step synthesis method prepares the method for nano-nickel-sulfur compound, and its specific steps are as follows:

[0049] (1) First, choline chloride and glycerol are placed in a beaker to mix uniformly according to a molar ratio of 1:3 to form a deep eutectic solvent as a solvent to be used;

[0050] (2) Then add a certain amount of 0.02mol / L nickel chloride, 0.04mol / L sodium thiosulfate and 0.01mol / L sublimed sulfur powder into the deep eutectic solvent, and stir at a temperature of 25°C until completely dissolve;

[0051] (3) Stir and heat the deep eutectic solvent in which nickel source, sulfur source and reactants are completely dissolved, the stirring speed is controlled at 100 rpm, the temperature is 110°C, and the reaction time is 6h;

[0052] (4) Finally, the generated powder is ultrasonically washed with distilled water, washed with alcohol, and dried in vacuum to obtain high-purity nano-NiS 2 pink.

[0053] The nano-NiS prepared ...

example 2

[0055] Deep eutectic solvent one-step synthesis method prepares the method for nano-nickel-sulfur compound, and its specific steps are as follows:

[0056] (1) choline chloride and propylene glycol are placed in a beaker to mix uniformly according to a molar ratio of 1:4 to form a deep eutectic solvent as a solvent to be used;

[0057] (2) Then add 0.05mol / L of nickel sulfate, 0.1mol / L of sodium thiosulfate and 0.005mol / L of ethylenediaminetetraacetic acid into the deep eutectic solvent, and stir at a temperature of 10°C until completely dissolved ,;

[0058] (3) Stir and heat the deep eutectic solvent that dissolves the nickel source, sulfur source, and reactants again, the stirring speed is controlled at 200 rpm, the temperature is 110°C, and the reaction time is 12h;

[0059] (4) Finally, the generated powder is ultrasonically washed with distilled water, washed with alcohol, and vacuum-dried to obtain high-purity nano-Ni 3 S 4 pink.

[0060] Ni was prepared in this exa...

example 3

[0062] Deep eutectic solvent one-step synthesis method prepares the method for nano-nickel-sulfur compound, and its specific steps are as follows:

[0063] (1) First, choline chloride and urea are placed in a beaker in a molar ratio of 1:2 and mixed evenly to form a deep eutectic solvent as a solvent to be used;

[0064] (2) Then add 0.1mol / L nickel acetate, 0.2mol / L thiourea and 0.05mol / L sublimed sulfur powder into the deep eutectic solvent, and stir at 0°C until completely dissolved;

[0065] (3) Stir and heat the fully dissolved eutectic solvent of nickel source, sulfur source, and reactant again, the stirring speed is controlled at 400 rpm, the temperature is 120°C, and the reaction time is 18h;

[0066] (4) The resulting powder can be ultrasonically washed with distilled water, washed with alcohol, and dried in vacuum to obtain NiS 2 and Ni 3 S 4 pink.

[0067] The XRD of the nano nickel sulfur compound that this example prepares is as follows Figure 7 shown.

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Abstract

The invention provides a method for preparing a nano nickel-sulfur compound based on a eutectic solvent one-step synthesis method. The method includes the steps of preparing a eutectic solvent; controlling the addition amount of a nickel source, a sulfur source and a reactant; adding the nickel source, the sulfur source and the reactant to the eutectic solvent to completely dissolve, thereby obtaining a eutectic solvent-nickel-sulfur system, wherein in the eutectic solvent-nickel-sulfur system, the nickel ion concentration is not less than 0.01 mol / L, the sulfur source concentration is not less than 0.01 mol / L, and the reactant concentration is not less than 0.01 mol / L. The eutectic solvent-nickel-sulfur system is heated and stirred, and after the reaction is completed, the product is taken out, washed, and dried to obtain a nano nickel-sulfur compound. The preparation method of the invention has the advantages of low equipment requirement, low temperature requirement, short process flow, controllable shape and size, and the like, the eutectic solvent used is environmentally friendly, simple in synthesis and low in price, and the method is an efficient and environment-friendly synthesis method.

Description

technical field [0001] The invention relates to the technical field of chemical material preparation, and more specifically, relates to a method for preparing nano-nickel-sulfur compounds by a one-step synthesis method in a deep eutectic solvent. Background technique [0002] Transition metal structure compound MX 2 (M=Mn, Fe, Co, Ni, etc., X=S, Se, Te, etc.), usually has a pyrite structure, has excellent optical, electrical, magnetic and catalytic properties, and has become the focus of material science research today. hotspot. Among these compounds, nickel-sulfur compounds have attracted increasing attention because of their unique electronic structure and excellent electrical and magnetic properties. etc. have broad industrial application prospects. [0003] At present, the methods for preparing nickel-sulfur compounds mainly include high-temperature solid-phase method, high-energy ball milling method, hydrothermal / solvothermal method, spray pyrolysis / drying method, et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/11B82Y40/00
CPCC01G53/11B82Y40/00C01P2002/72C01P2004/03C01P2002/85C01P2004/64C01P2004/62C01P2006/80
Inventor 汝娟坚张远华一新
Owner KUNMING UNIV OF SCI & TECH
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