Preparation method of metal sulfide

A technology of metal sulfide and metal ions, applied in chemical instruments and methods, copper sulfide, zinc sulfide, etc., can solve the problems of environmental pollution, S2- entering the atmosphere or water, etc., and achieve large specific surface area, high yield, and structure Unit Controllable Effects

Inactive Publication Date: 2020-07-03
ZHEJIANG UNIV
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  • Description
  • Claims
  • Application Information

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Although it can be post-processed, there will still be a sma...

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  • Preparation method of metal sulfide
  • Preparation method of metal sulfide
  • Preparation method of metal sulfide

Examples

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Embodiment 1

[0027] 1) Add 0.320g of thiocyanuric acid to 5ml of DMF, and stir at room temperature until a yellow clear and transparent solution is formed, which is designated as solution A;

[0028] 2) 0.450g nickel acetate tetrahydrate (Ni(CH 3 COO) 2 4H 2 O) added to 5ml of DMF, stirred at 50°C until a clear solution was formed, which was designated as solution B;

[0029] 3) With stirring at room temperature, add solution A dropwise to solution B, and the solution immediately becomes turbid, accompanied by continuous precipitation of brown precipitates;

[0030] 4) The above-mentioned brown precipitate was collected by vacuum filtration, washed three times with distilled water and ethanol, and then dried at a constant temperature of 60° C. under vacuum conditions for 12 hours;

[0031] 5) heat treatment is carried out to the precipitate after drying, and the heat treatment process is: in N 2 Heat up to 600°C at a rate of 5°C / min in the atmosphere, keep warm for 2 hours and then coo...

Embodiment 2

[0034] 1) Add 0.320g of thiocyanuric acid to 5ml of DMF, stir vigorously at 30°C until a yellow clear and transparent solution is formed, which is designated as solution A

[0035] 2) 0.450g cobalt acetate tetrahydrate (Co(CH 3 COO) 2 4H 2 O) added to 5ml of DMF, stirred vigorously at 50°C until a clear solution was formed, which was designated as solution B;

[0036] 3) Stir at 30°C, add solution A dropwise to solution B, the solution immediately becomes turbid, accompanied by continuous precipitation of brown precipitates (the ratio of Co to S is 1:1);

[0037] 4) The above-mentioned brown precipitate was subjected to vacuum filtration, washed three times with distilled water and ethanol, and then dried at 60° C. under constant temperature and vacuum conditions for 12 hours;

[0038] 5) heat treatment is carried out to the precipitate after drying, and the heat treatment process is: in N 2 In the atmosphere, the temperature is raised to 500°C at a rate of 10°C / min, and a...

Embodiment 3

[0041] 1) Add 0.320g of thiocyanuric acid to 5ml of DMF, and stir vigorously at 40°C until a yellow clear and transparent solution is formed, which is designated as solution A

[0042] 2) 0.396g zinc acetate dihydrate (Zn(CH 3 COO) 2 2H 2 O) add it to 5ml of DMF, and stir vigorously at 50°C until a clear solution is formed, which is referred to as solution B;

[0043] 3) Stir at 40°C, add solution A drop by drop to solution B, the solution immediately becomes turbid, accompanied by continuous precipitation of white precipitates (the ratio of the amount of Zn to S is 1:1);

[0044] 4) The above-mentioned white precipitate was subjected to vacuum filtration, washed three times with distilled water and ethanol, and then dried at a constant temperature of 60° C. under vacuum conditions for 12 hours;

[0045] 5) heat treatment is carried out to the precipitate after drying, and the heat treatment process is: in N 2 In the atmosphere, the temperature was raised to 400°C at a rat...

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Abstract

The invention discloses a preparation method of metal sulfide. The preparation method comprises the following steps: 1) dissolving trithiocyanuric acid in dimethyl formamide to obtain a solution A; 2)dissolving metal acetate in DMF to obtain a solution B; 3) dropwise adding the solution A into the solution B under ultrasonic waves or stirring to obtain a precipitate; and 4) carrying out a heat treatment on the precipitate to obtain corresponding metal sulfide. The general formula of the chemical components of the metal sulfide is MxSy, M can be any one of Co, Ni, Cu, Zn, Ag and Cd or combination of several of Co, Ni, Cu, Zn, Ag and Cd in any proportion, and S is sulfur. Test results show that prepared metal sulfide is an aggregate of nano/submicron particles, and is high in purity and good in crystallinity. The disclosed preparation method is easy to operate, low in time consumption and high in yield, takes trithiocyanuric acid as a sulfur source, and has the characteristics of environmental friendliness and wide source.

Description

technical field [0001] The invention belongs to the technical field of metal sulfide material preparation, and in particular relates to a process for preparing metal sulfide. Background technique [0002] Transition metal sulfides (TMS) have attracted much attention due to their excellent physical and chemical properties, and are widely used in various fields such as catalysis, energy, environment, and optoelectronics. For example, since M x S y It can react with lithium ions and lithium ions can be in the layered MS 2 Therefore, TMS material has a higher theoretical specific capacity than graphene, making it one of the main candidate materials for lithium battery cathode materials. TMS has a polar sulfophilic surface, which has a strong affinity with soluble polysulfides, avoiding the dissolution of lithium (poly)sulfides in the electrolyte during discharge, which is beneficial for its use as a high-efficiency electrode for lithium-sulfur batteries. 2D MS 2 With strong...

Claims

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Application Information

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IPC IPC(8): C01G53/11C01G53/00C01G51/00C01G11/02C01G9/08C01G5/00C01G3/12
CPCC01G3/12C01G5/00C01G9/08C01G11/02C01G51/30C01G53/006C01G53/11C01P2002/72C01P2004/03C01P2004/50C01P2004/62
Inventor 洪樟连欧阳冲支明佳
Owner ZHEJIANG UNIV
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