Nickel-cobalt disulfide composite material and preparation method and application thereof

A technology of disulfide and composite materials, applied in chemical instruments and methods, chemical/physical process, physical/chemical process catalyst, etc., can solve the problems of poor process feasibility, difficult product separation, high energy consumption, etc. The effect of liquid separation, good electrocatalytic performance and high process feasibility

Active Publication Date: 2020-05-08
赛帝迦(山东)科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. The process of preparing disulfides by the solid phase method is efficient and fast, but it is not easy to control the product morphology and active sites, and it is difficult to control the performance of the material;
[0006] 2. In water-based hydrothermal research, disulfides with high activity are prone to oxidation in the presence of water and oxygen, forming sulfate or oxides, and the stability of material properties is poor;
[0007] 3. In the organic high-temperature wet synthesis process, researchers usually use ethylene glycol as a solvent. On the one hand, it can dissolve the transition metal nickel source, and on the other hand, it can use its own viscous properties to form a suspension of sulfur. However, this experiment There are huge problems, one is that ethylene glycol is highly toxic to the human body; the other is that the smell is heavy after the test, and the working environment is poor; the third is that the viscosity of ethylene glycol is high, the product separation is difficult, and the process feasibility is poor; the fourth is the reaction temperature high, high energy consumption

Method used

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  • Nickel-cobalt disulfide composite material and preparation method and application thereof
  • Nickel-cobalt disulfide composite material and preparation method and application thereof
  • Nickel-cobalt disulfide composite material and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1 A kind of nickel disulfide material preparation method

[0028] Weigh the nickel source Ni(CHCOO) according to the stoichiometric ratio of 1:10 2 4H 2 O (0.25g) and sublimed sulfur (0.32g) were added into a beaker with 15mL of ethanol and 20mL of DMF organic solvent, and the stirring speed was controlled at 600r / min to mix the raw materials for 30min to form a suspension. The resulting suspension after mixing was transferred to a 50 mL Teflon-lined stainless steel autoclave. After sealing, place it in a blast drying oven, and react in a high-temperature environment of 160°C for 24 hours. After the reaction was completed, it was naturally cooled to room temperature and centrifuged to obtain a black product, which was washed several times with a mixed organic reagent of ethanol and carbon disulfide, filtered to obtain a black powder nickel-cobalt disulfide composite material, and dried at 60°C for 12 hours. through figure 1 The XRD pattern and figure 2A...

Embodiment 2

[0029] Embodiment 2 A kind of preparation method of cobalt disulfide material

[0030] Weigh the cobalt source Co(CHCOO) respectively according to the stoichiometric ratio of 1:12 2 4H 2 O (0.25g) and sublimed sulfur (0.38g) were added to a beaker with 20mL of ethanol and 15mL of DMF organic solvent, and the stirring speed was controlled at 600r / min to mix the raw materials for 45min to form a suspension. The resulting suspension after mixing was transferred to a 50 mL Teflon-lined stainless steel autoclave. After sealing, place it in a blast drying oven, and react in a high-temperature environment of 160°C for 24 hours. After the reaction was completed, it was naturally cooled to room temperature and centrifuged to obtain a black product, which was washed several times with a mixed organic reagent of ethanol and carbon disulfide, filtered to obtain a black powder nickel-cobalt disulfide composite material, and dried at 60°C for 12 hours. through figure 1 The XRD pattern a...

Embodiment 3

[0031] Embodiment 3 A kind of nickel-cobalt disulfide composite material preparation method

[0032] Weigh the nickel source Ni(CHCOO) according to the stoichiometric ratio of 1:1:20 2 4H 2 O (0.13g), cobalt source Co (CHCOO) 2 4H 2 O (0.13g) and sublimed sulfur (0.32g) were added to a beaker with 15mL of ethanol and 20mL of DMF organic solvent, and the stirring speed was controlled at 600r / min to mix the raw materials for 1h to form a suspension. The resulting suspension after mixing was transferred to a 50 mL Teflon-lined stainless steel autoclave. After sealing, place it in a blast drying oven, and react in a high-temperature environment of 160°C for 24 hours. After the reaction was completed, it was naturally cooled to room temperature and centrifuged to obtain a black product, which was washed several times with a mixed organic reagent of ethanol and carbon disulfide, filtered to obtain a black powder nickel-cobalt disulfide composite material, and dried at 60°C for 1...

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Abstract

The invention discloses a nickel-cobalt disulfide composite material and a preparation method and application thereof. The preparation method comprises the following steps: dissolving a nickel source,a cobalt source and elemental sulfur in an organic solvent under stirring to obtain turbid liquid; transferring the turbid liquid into a reaction container; after sealing, carrying out reacting for 1to 24 h at 120 to 200 DEG C; and carrying out solid-liquid separation, washing, filtering and drying to obtain the nickel-cobalt disulfide composite material. The phase of the nickel-cobalt disulfidecomposite material is cobalt disulfide (CoS<2>), nickel disulfide (NiS<2>) or a cobalt-nickel disulfide composite phase (Ni<x>Co<1-x>S<2>). According to the method, required equipment is simple, preparation cost is low, and used raw materials are green, non-toxic and environment-friendly; and the method provided by the invention is simple to operate and controllable in conditions, particularly, no solvent with high viscosity is adopted, solid-liquid separation is easy, and process feasibility is high.

Description

technical field [0001] The invention relates to the technical field of water splitting electrocatalysis, and more specifically relates to a nickel-cobalt disulfide composite material and its preparation method and application. Background technique [0002] With the increase of fossil fuel consumption, energy crisis and environmental pollution have become social problems that need to be solved urgently. Finding an alternative clean energy source is the current main research direction, and hydrogen, as a clean and sustainable fuel, is considered to be the most promising alternative to fossil fuels. Hydrogen production by electrolysis of water is one of the ways, which can not only obtain pollution-free and sustainable hydrogen energy, but also produce usable high-purity oxygen. [0003] However, the key to hydrogen production from water electrolysis is to develop high-efficiency electrocatalysts to reduce the excess energy consumption of electricity. To date, the most effici...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/049B01J35/00B01J35/08C25B1/04C25B11/06H01M4/90
CPCB01J27/049B01J35/0033B01J35/08H01M4/9083C25B1/04C25B11/091Y02E60/36Y02E60/50
Inventor 韩晓鹏田千秋胡文彬向文帝邓意达钟澄
Owner 赛帝迦(山东)科技有限公司
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