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New method for two-step process preparation of nickel sulfide

A nickel sulfide, step method technology, applied in nickel sulfide and other directions, can solve problems such as the wide application of unfavorable nickel sulfide micro-nano materials, environmental pollution, etc., and achieve stable and reliable product performance, no environmental pollution, and good consistency.

Inactive Publication Date: 2015-01-07
XUZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods have obtained nickel sulfide materials with uniform morphology, but a large amount of H2S is generated in the process, causing serious environmental pollution, which is not conducive to the wide application of nickel sulfide micro-nano materials

Method used

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  • New method for two-step process preparation of nickel sulfide
  • New method for two-step process preparation of nickel sulfide
  • New method for two-step process preparation of nickel sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dissolve 2.5 mmol nickel chloride in 35 mL deionized water, add 10 mmol urea, then transfer to an autoclave, heat at 120 °C for 16 h, cool naturally, filter, wash the product, and dry it at 60 °C The nickel hydroxide precursor can be obtained in 12 h. Weigh 0.3 g of nickel hydroxide precursor, ultrasonically disperse (100 W power, 15 minutes) into 50 mL of ethylene glycol, then add 10 mL of aqueous solution containing 5 g of sodium sulfide nonahydrate, and dissolve the above mixed solution Transfer to a 100 mL round bottom flask, place in an oil bath, condense and reflux at 160 °C for 12 h, cool naturally, wash the obtained black precipitate with water and absolute ethanol (three times each), and then Nickel sulfide can be obtained by drying at 60 °C for 12 h.

[0032] Such as figure 1 As shown, the obtained precursor is Ni(OH)2 ((JCPDS Card.14-117).

[0033] Such as figure 2 As shown, the composition of the obtained nickel sulfide is pure phase Ni3S4 ((JCPDS Card....

Embodiment 2

[0037] Dissolve 2.5 mmol of nickel chloride in 30 mL of deionized water, add 2 mL of ammonia water, then transfer to an autoclave, heat at 160 °C for 8 h, cool naturally, wash the product, and dry at 60 °C for 12 h A nickel hydroxide precursor can be obtained. Weigh 0.3 g of nickel hydroxide precursor, ultrasonically disperse (100 W power, 16 minutes) into 50 mL of ethylene glycol, then add 10 mL of aqueous solution containing 5 g of sodium sulfide nonahydrate, and dissolve the above mixed solution Transfer to a 100 mL round-bottomed flask, place in an oil bath, condense and reflux at 160 °C for 24 h, after natural cooling, wash the obtained black precipitate with water and absolute ethanol (washing three times each), and in Nickel sulfide can be obtained by drying at 60 °C for 12 h.

[0038] Such as Figure 5 As shown, the prepared nickel sulfide is composed of microspheres with a diameter of about 3 μm, and the microspheres have a flower-like structure.

Embodiment 3

[0040] Dissolve 2.5 mmol of nickel chloride in 25 mL of ethylene glycol, add 10 mL of deionized water to 2 mL of ammonia water, mix the two solutions slowly, transfer to an autoclave, heat at 160 °C for 16 h, and cool naturally , the product was washed and dried at 60 °C for 12 h to obtain the nickel hydroxide precursor. Weigh 0.3 g of nickel hydroxide precursor, ultrasonically disperse (100 W power, 16 minutes) into 50 mL of ethylene glycol, then add 10 mL of aqueous solution containing 5 g of sodium sulfide nonahydrate, and dissolve the above mixed solution Transfer to a 100 mL round-bottomed flask, place in an oil bath, condense and reflux at 160 °C for 16 h, and after natural cooling, wash the obtained black precipitate with water and absolute ethanol (three times each), and in Nickel sulfide can be obtained by drying at 60 °C for 12 h.

[0041] Such as Figure 6 As shown, the prepared nickel sulfide is composed of hexagonal sheets with uniform shape and side length of a...

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Abstract

The invention relates to a new method for two-step process preparation of nickel sulfide. The new method comprises the following steps: transferring a water and urea mixed solution of nickel chloride or a water, ammonia water and ethylene glycol mixed solution of nickel chloride into a high-pressure kettle, performing heating reaction at the temperature of 120-160 DEG C for 8-16h, filtering and washing a generated nickel hydroxide precipitate, and drying to prepare a nickel hydroxide precursor; and then dispersing into ethylene glycol, performing ultrasonic dispersion, adding sodium sulfide nonahydrate, transferring into a reactor, performing reflux reaction at the temperature of 160 DEG C for 12-24h, filtering, washing, and performing vacuum drying for 10-12h to prepare nickel sulfide. The new method provided by the invention has the advantages of simple production process, easiness in control of reaction conditions, no need of using a template agent and a surfactant, environmental friendliness and good consistency of the obtained product, is conductive to production of nickel sulfide, and has important practical significance.

Description

technical field [0001] The invention relates to a new method for preparing nickel sulfide by a two-step method, in particular to a method for preparing nickel sulfide by a two-step method of hydrothermal-condensation reflux. Background technique [0002] In recent years, nickel sulfide has attracted extensive research interest due to its excellent optical, electrical, and catalytic properties, and has been successfully used in various fields, such as industrial catalysts, semiconductor materials, optoelectronic materials, and lithium-ion battery negative electrode materials. and supercapacitor materials. Studies have shown that the physical and chemical properties of materials are closely related to the structure and size of materials. Therefore, more and more research focuses on the controllable synthesis of nickel sulfide materials with certain shapes, sizes and dimensions. [0003] Most of the traditional preparation methods of nickel sulfide involve multiphase reaction...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/11
Inventor 王庆红杨加芹王庆鹏陈娟陈丹杜佳璐朱丽璇
Owner XUZHOU NORMAL UNIVERSITY
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