Preparation method of iron disulfide microspheres

A technology of ferrous disulfide and microspheres, applied in the direction of iron sulfide, etc., to achieve the effects of cheap and easy-to-obtain raw materials, simple equipment, and easy control.

Active Publication Date: 2011-11-23
LANZHOU LANSHI ZHONGKE NANOTECHNOLOGY CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report on the preparation method of uniformly dispersed pyrite-type ferrous disulfide microspheres

Method used

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  • Preparation method of iron disulfide microspheres
  • Preparation method of iron disulfide microspheres
  • Preparation method of iron disulfide microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take by weighing 1mmol analysis pure ferric trichloride hexahydrate, 0.3g urea joins in the stainless steel pressure-resistant reactor of the polytetrafluoro liner of the mixed solution that 35mL ethylene glycol and nitrogen, nitrogen dimethylformamide are formed in 50 mL), stirred to obtain a clear homogeneous solution. Then react at 160° C. for 12 hours in a closed reactor. Then cool to room temperature, open the reactor, centrifuge the black precipitate at the bottom of the reactor, wash with deionized water, and dry to obtain a black powder. The product is identified as cubic phase by X-ray powder diffraction; characterized by field emission scanning electron microscopy, the product is in the shape of uniformly dispersed microspheres, and the particle size is about 4 microns.

Embodiment 2

[0018] Weigh 1mmol of analytically pure ferric chloride hexahydrate, and add it to a stainless steel pressure-resistant reactor with a polytetrafluoro liner (volume 50mL) that contains 35mL of a mixed solution of ethylene glycol, nitrogen, and nitrogen dimethylformamide. , stirred to obtain a clear homogeneous solution. Then react at 160° C. for 12 hours in a closed reactor. Then cool to room temperature, open the reactor, centrifuge the black precipitate at the bottom of the reactor, wash with deionized water, and dry to obtain a black powder. The product is identified as cubic phase by X-ray powder diffraction; characterized by field emission scanning electron microscopy, the product is in the shape of uniformly dispersed microspheres, and the particle size is about 4 microns.

Embodiment 3

[0020] Weigh 1mmol of analytically pure ferric chloride hexahydrate, and add it to a stainless steel pressure-resistant reactor with a polytetrafluoro liner (volume 50mL) that contains 35mL of a mixed solution of ethylene glycol, nitrogen, and nitrogen dimethylformamide. , stirred to obtain a clear homogeneous solution. Then react at 170° C. for 12 hours in a closed reactor. Then cool to room temperature, open the reactor, centrifuge the black precipitate at the bottom of the reactor, wash with deionized water, and dry to obtain a black powder. The product is identified as cubic phase by X-ray powder diffraction; characterized by field emission scanning electron microscopy, the product is in the shape of uniformly dispersed microspheres, and the particle size is about 4 microns.

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Abstract

The invention discloses a preparation method of iron disulfide microspheres. Specifically, the method comprises the steps of: dissolving iron chloride, or iron chloride and urea in a mixed solution consisting of ethylene glycol and N,N-dimethylformamide, thus obtaining a clear homogeneous solution containing iron ions; adding sulfur powder; subjecting the mixed solution to a reaction for 10-20h at a temperature of 150-170DEG C, conducting separation with a conventional method, thus obtaining black powder, i.e. pyrite-type monodispersed iron disulfide microspheres. Products obtained with the method of the invention have uniform particle size and appearance, good technological repeatability and stable quality. Thus, the method provided in the invention is expected to be applied in the fields of solar energy conversion, heavy metal ion fixation, etc.

Description

technical field [0001] The invention relates to a synthesis method of transition metal sulfides, in particular to a preparation method of pyrite-type ferrous disulfide uniformly dispersed microspheres, which belongs to the field of inorganic chemical industry. Background technique [0002] Pyrite-type ferrous disulfide is widely used in photovoltaic solar cells, lithium-ion battery electrode materials and other fields due to its unique optical and electrical properties. In addition, pyrite also plays a key role in primary ore separation and coal separation. Existing preparation methods mainly rely on the decomposition of single source precursors (SSPs), but the products often contain residues of impurities and surfactants. For example, the group of Professor Alivisatos recently obtained single-phase pyrite crystals by hydrothermally decomposing single-source precursors with the aid of surfactants, but the products have serious surfactant residues (Chem.Mater., 2009, 21, 2568...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/12
Inventor 王齐华汪德伟王廷梅
Owner LANZHOU LANSHI ZHONGKE NANOTECHNOLOGY CO LTD
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