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Preparation method and application of hollow MoS2 microspheres

A microsphere, hollow technology, applied in chemical instruments and methods, other chemical processes, molybdenum sulfide, etc., can solve the problems of less MoS2 material, ultra-thin nanosheet separation, difficulty in collection, limited application, etc., and achieve rich reactive sites. point, convenient for industrial application, uniform particle size effect

Active Publication Date: 2019-04-19
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the reported MoS2 materials are ultrathin nanosheet structures, while MoS2 with other structural morphologies 2 Materials are less reported
At the same time, due to the difficulty in separating and collecting ultra-thin nanosheets in actual use, their wide application is limited.

Method used

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  • Preparation method and application of hollow MoS2 microspheres
  • Preparation method and application of hollow MoS2 microspheres
  • Preparation method and application of hollow MoS2 microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Add 4.054g of ferric chloride hexahydrate (FeCI 3 ·6H 2 O) and 1.2g of hexamethylenetetramine (HMT) were added into a beaker equipped with 30ml of ethanol / water mixed solvent with a volume ratio of 1:1, and stirred to completely dissolve it. Then add 1.0wt% copper nitrate trihydrate (Cu(NO 3 ) 2 ·3H 2 0), after stirring for 30min, the solution was transferred to a 50ml hydrothermal reaction kettle, after 180°C hydrothermal reaction for 24h, the sample was taken out after cooling, washed with absolute ethanol and deionized water, centrifuged, and finally put into a drying box for 80 Dry at ℃ for 10h to obtain Cu-α-Fe 2 o 3 as a template.

[0030] 2) Add 0.35g ammonium molybdate tetrahydrate ((NH 4 )6Mo 7 o 24 4H 2 O), 0.76g thiourea (CN 2 h 4 S) was dissolved in 20ml deionized water, and stirred with magnetic force for 30min to make it completely dissolved, then added 20mg of Cu-α-Fe obtained 2 o 3 , stir for 30 minutes to make it completely dispersed, t...

Embodiment 2

[0040] 1) 2.1g of ferric chloride hexahydrate (FeCl 3 ·6H 2 O) and 1.5g of hexamethylenetetramine (HMT) were added into a beaker equipped with 30ml of ethanol / water mixed solvent with a volume ratio of 1:1, and stirred to completely dissolve it. Then add 3.0wt% copper nitrate trihydrate (Cu(NO 3 ) 2 ·3H 2 0), after stirring for 30min, the solution was transferred to a 50ml hydrothermal reaction kettle, after 180°C hydrothermal reaction for 24h, the sample was taken out after cooling, washed with absolute ethanol and deionized water, centrifuged, and finally put into a drying box for 80 Dry at ℃ for 10h to obtain Cu-α-Fe 2 o 3 as a template.

[0041] 2) Add 0.5g ammonium molybdate tetrahydrate ((NH 4 )6Mo 7 o 24 4H 2 O), 0.8g thiourea (CN 2 h 4 S) was dissolved in 20ml deionized water, and stirred with magnetic force for 30min to make it completely dissolved, then added 20mg of Cu-α-Fe obtained 2 o 3 , stir for 30 minutes to make it completely dispersed, then add ...

Embodiment 3

[0051] 1) Add 3g of ferric nitrate and 1.5g of hexamethylenetetramine (HMT) into a beaker filled with 50ml of ethanol / water mixed solvent with a volume ratio of 1:2, and stir to dissolve them completely. Then add 2.0wt% copper nitrate trihydrate (Cu(NO 3 ) 2 ·3H 2 0), after stirring for 30min, the solution was transferred to a 50ml hydrothermal reaction kettle, after 160°C hydrothermal reaction for 20h, the sample was taken out after cooling, washed with absolute ethanol and deionized water, centrifuged, and finally put into a drying box for 80 Dry at ℃ for 10h to obtain Cu-α-Fe 2 o 3 as a template.

[0052] 2) Add 0.5g ammonium molybdate tetrahydrate ((NH 4 )6Mo 7 o 24 4H 2 O), 0.8g thiourea (CN 2 h 4 S) was dissolved in 20ml deionized water, and stirred with magnetic force for 30min to make it completely dissolved, then added 20mg of Cu-α-Fe obtained 2 o 3 , stir for 30 minutes to make it completely dispersed, then add it to a 50mL hydrothermal reaction kettle, a...

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Abstract

The invention provides large-sized hollow MoS2 microspheres with surface porous structures and a preparation method and application of the microspheres. The preparation method comprises the steps thatfirstly, large-sized Cu-Fe2O3 microspheres are prepared by means of a hydrothermal method, secondly, MoS2 layered nanosheets perpendicularly grow on the surfaces of the microspheres with the microspheres as a template by means of the hydrothermal method, and finally, a template in an obtained composite material is removed by means of a corrosion etching solution etching method to obtain the large-sized hollow MoS2 microspheres. It is shown by a result of the embodiment that the large-sized hollow MoS2 microspheres can be prepared, and the size distribution is 1-30 micron; the surfaces of thehollow microspheres are provided with the porous structure assembled with the ultra-thin nanosheets, the MoS2 microspheres have the abundant pore structures, pores are mesopores and macropores with the size of 2-500 nm, and the thickness of a shell layer can be adjusted within 5-500 nm. The prepared MoS2 material is large in size, nanosheet-shaped molybdenum disulfide perpendicularly grows and isarrayed to form a three-dimensional porous structure, and the large-sized hollow MoS2 microspheres have excellent performance in the fields of catalysis, photo / electrocatalysis, adsorption, gas-sensitive induction, lubrication and the like.

Description

technical field [0001] This technology belongs to the field of preparation of two-dimensional layered materials, and the technology involves hydrothermal method, especially a large-sized hollow MoS 2 Microspheres and methods of preparation and applications thereof. Background technique [0002] Since the discovery of graphene, two-dimensional layered materials have attracted extensive attention in recent years due to their excellent optical, electrical, magnetic and mechanical properties. Among them, the transition metal sulfide has the structural characteristics of graphene. The metal W / Mo atomic layer is sandwiched by two S / Se atomic layers, forming a typical sandwich structure. The layers are combined by strong chemical bonds, and the layers They are combined by weak van der Waals force, which is a typical inorganic layered compound. Transition metal dichalcogenides (TMDs) have become a hot topic due to their unique properties, and have been widely used in many fields s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B01J20/02B01J20/30B01J27/051
CPCB01J20/0218B01J20/0285C01G39/06B01J27/051C01P2002/84C01P2002/72C01P2004/34C01P2004/04C01P2004/03C01P2004/61C01P2006/12B01J35/33
Inventor 乔秀清李东升侯东芳赵君
Owner CHINA THREE GORGES UNIV
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