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Universal method for preparing nano metal sulfides and complexes thereof in one step

A general method and nano metal technology, applied in the field of nano materials, can solve the problems of increasing the production cost of nano metal sulfides, increasing the cost of wastewater treatment, high reaction temperature, etc., and achieving the effects of low cost, reduced production cost and high safety.

Active Publication Date: 2018-10-19
SOUTHWEST UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the patent CN 1911787A requires a higher reaction temperature and the use of carcinogenic thiourea, and the patent CN10185726 5A requires the use of long-chain mercaptans. After the reaction is completed, there will be organic matter, which increases the cost of wastewater treatment. The patent CN 102633297A discloses The method requires a specific organic sulfur metal salt, and a large amount of organic matter will be produced after the production is completed, which greatly increases the production cost of nano-metal sulfides

Method used

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  • Universal method for preparing nano metal sulfides and complexes thereof in one step

Examples

Experimental program
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Effect test

Embodiment 1

[0032] A kind of preparation Bi 2 S 3 The method for nanosheet, is characterized in that, comprises the steps:

[0033] (1) Solution preparation: Bi 2 o 3 powder, sublimed sulfur powder and oxalic acid powder were added to deionized water, where Bi 2 o 3 The powder and oxalic acid powder can be dissolved, and the sublimated sulfur powder is uniformly dispersed in the solution, and then the three solutions are mixed, and the concentration of each substance after mixing is 0.0125mol / L, 0.0375mol / L and 0.1125mol / L respectively.

[0034] (2) Reaction: Put the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, and make the volume of the mixed solution account for 60-80% of the total capacity, and then put the reaction kettle into a medium oven at 220°C for reaction 24 hours; after the reaction was completed, the reactor was taken out, and air-cooled to room temperature.

[0035] (3) Sample treatment: Take out the cooled solution, centrifuge at 12000r...

Embodiment 2

[0038] A preparation of NiS 2 The method of micron square is characterized in that, comprises the steps:

[0039] (1) Solution preparation: dissolve NiCl respectively 2 ·6H 2 O powder, sublimed sulfur powder and oxalic acid powder in deionized water, where NiCl 2 ·6H 2 O powder and oxalic acid powder can be dissolved, sublimated sulfur powder is uniformly dispersed in the solution, and then the solutions are mixed, and the concentration of each substance after mixing is respectively 0.025mol / L, 0.025mol / L and 0.025mol / L.

[0040] (2) Reaction: Put the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, and make the volume of the mixed solution account for 60-80% of the total capacity, and then put the reaction kettle into a medium oven at 220°C for reaction 24 hours; after the reaction was completed, the reactor was taken out, and air-cooled to room temperature.

[0041] (3) Sample treatment: Take out the cooled solution, centrifuge at 10000rpm fo...

Embodiment 3

[0044] A method for preparing NiS micron square, is characterized in that, comprises the steps:

[0045] (1) Solution preparation: dissolve NiCl respectively 2 ·6H 2 O powder, sublimed sulfur powder and oxalic acid powder in deionized water, where NiCl 2 ·6H 2 The O powder and the oxalic acid powder can be dissolved, and the sublimated sulfur powder is evenly dispersed in the solution, and then the solutions are mixed, and the concentration of each substance after mixing is respectively 0.025mol / L, 0.025mol / L and 0.075mol / L.

[0046] (2) Reaction: Put the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, and make the volume of the mixed solution account for 60-80% of the total capacity, and then put the reaction kettle into a medium oven at 220°C for reaction 24 hours; after the reaction was completed, the reactor was taken out, and air-cooled to room temperature.

[0047] (3) Sample treatment: Take out the cooled solution, centrifuge at 10000rpm...

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Abstract

The invention relates to the field of nano-materials and particularly relates to a universal method for preparing nano metal sulfides and complexes thereof in one step. According to the universal method, nano metal sulfides are subjected to hydrothermal synthesis by adopting elemental sulfur as a sulfur source, adopting oxalic acid as a reducer and adopting a metal oxide or metal salt as a metal source. According to the method, sulfur powder is directly adopted as the sulfur source without using organic sulfur as the sulfur source, so that the cost is lower, and the safety is higher; meanwhile, the oxalic acid with stable properties is adopted as the reducer, water serves as a solvent, and preparation can be carried out in relatively moderate environments, so that the safety of a preparation process is further improved, and the production cost is further reduced.

Description

technical field [0001] The invention relates to the field of nanometer materials, in particular to a general method for preparing nanometer metal sulfides and their composites in one step. Background technique [0002] The family of nano-metal sulfides contains both conductors, insulators, and semiconductors with tunable band gaps (such as CdS and ZnS), which have attracted extensive attention and continuous research by researchers in the past two decades. Various nano-metal sulfides have their unique properties. On the one hand, researchers explore the basic characteristics of specific materials, and on the other hand, conduct applied research on them, such as Huang et al. (Angew.Chem.Int.Ed., 2017, 56, 16583-16587) studied the electron transport properties of PbS / CdS core-shell quantum dots, Lee et al. (Adv. 2 As an oxygen catalyst in zinc-oxygen batteries, while Song et al. (Chem, 2018, 4, 162–173) investigated the ability of ZnS-CdS multilayer nanocages for photocatalyt...

Claims

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Application Information

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IPC IPC(8): C01B17/20C01G29/00C01G53/11B82Y40/00B82Y30/00
CPCB82Y30/00B82Y40/00C01B17/20C01G29/00C01G53/11C01P2002/72C01P2002/85C01P2004/03
Inventor 林华贺世杰覃礼钊邹建
Owner SOUTHWEST UNIVERSITY
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