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A kind of preparation method of highly dispersed nickel modified molybdenum disulfide

A molybdenum disulfide, highly dispersed technology, applied in the direction of molybdenum sulfide, liquid chemical plating, metal material coating process, etc.

Active Publication Date: 2021-09-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, usually the Ni / Co metal in this type of material is easy to agglomerate and cannot be well dispersed in the molybdenum disulfide material (Adv.Mater.2006,18(19),2561-2564.), and the introduced metal ions cannot be well dispersed. A good entry into the molybdenum disulfide lattice does not serve the purpose of changing the structure of the molybdenum disulfide material, or the catalyst is more effective in generating a more active bimetallic sulfur cluster compound

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  • A kind of preparation method of highly dispersed nickel modified molybdenum disulfide
  • A kind of preparation method of highly dispersed nickel modified molybdenum disulfide

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Experimental program
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Effect test

Embodiment 1

[0016] Use MoO 3 (3 mmol of) a molybdenum precursor, was added thioacetamide (21 mmol), deionized water was added, the mixture was adjusted to 200 mL volume, the reaction was stirred at room temperature for 2h. Then transferred to 300mL synthesis reactor, the synthesis reactor interior was replaced with nitrogen gas, sealed pot synthesis, hydrothermal synthesis 36h and then at 170 ℃. After completion of the reaction, it was filtered, washed with deionized water to give a sample, and dried in vacuo at 100 deg.] C, the sample is obtained, numbered MoS 2 (MoO-7-170-36) -A. ASAP 2010 instrument using physical adsorption measurement sample Micromeritics specific surface area of ​​the sample prior to testing at 110 deg.] C in vacuo for 3h above, a vacuum degree of 10 -6 About torr, then tested at liquid nitrogen temperature (-196 ℃), BET specific surface area is calculated using the equation. Nitrogen adsorption and desorption experiments indicates that the material specific surface are...

Embodiment 2

[0018] Use MoO 3 (3 mmol of) a molybdenum precursor added Dithiooxamide (15mmol), deionized water was added, the mixture was adjusted to 200 mL volume, the reaction was stirred at room temperature for 2h. Then transferred to 300mL synthesis reactor, the synthesis reactor interior was replaced with nitrogen gas, sealed pot synthesis, hydrothermal synthesis 36h and then at 170 ℃. After completion of the reaction, it was filtered, washed with deionized water to give a sample, and dried in vacuo at 100 deg.] C, the sample is obtained, numbered MoS 2 (MoO-10-170-36) -B. ASAP 2010 instrument using physical adsorption measurement sample Micromeritics specific surface area of ​​the sample prior to testing at 110 deg.] C in vacuo for 3h above, a vacuum degree of 10 -6 About torr, then tested at liquid nitrogen temperature (-196 ℃), BET specific surface area is calculated using the equation. Nitrogen adsorption and desorption experiments indicates that the material specific surface area of ...

Embodiment 3

[0020] Use MoO 3 (3 mmol of) a molybdenum precursor, thioacetamide (30mmol), deionized water was added, the mixture was adjusted to 200 mL volume, the reaction was stirred at room temperature for 2h. Then transferred to 300mL synthesis reactor, the synthesis reactor interior was replaced with nitrogen gas, sealed pot synthesis, hydrothermal synthesis and then 24h at 180 ℃. After completion of the reaction, it was filtered, washed with deionized water to give a sample, and dried in vacuo at 100 deg.] C, the sample is obtained, numbered MoS 2 (MoO-10-180-24) -A. ASAP 2010 instrument using physical adsorption measurement sample Micromeritics specific surface area of ​​the sample prior to testing at 110 deg.] C in vacuo for 3h above, a vacuum degree of 10 -6 About torr, then tested at liquid nitrogen temperature (-196 ℃), BET specific surface area is calculated using the equation. Nitrogen adsorption and desorption experiments indicates that the material specific surface area of ​​85m...

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Abstract

The invention relates to a preparation method of highly dispersed nickel-modified molybdenum disulfide. The method firstly disperses the molybdenum-containing and sulfur-containing precursors into the same solution according to the atomic ratio of Mo:S=1:4~1:60, and then transfers the solution to a hydrothermal synthesis kettle, at 140~220 Under the condition of ℃, react for 6-48 hours, centrifuge, wash and dry in vacuum to obtain molybdenum disulfide material with coordination unsaturated Mo center. The obtained molybdenum disulfide material having a coordinatively unsaturated Mo center is dispersed in an aqueous solution of nickel formate according to the atomic ratio of Ni:Mo=1:1000~1:20, and then the mixture is transferred to a hydrothermal synthesis tank , treated at 120-200°C for 3-48 hours, and the solid obtained by centrifugal washing is highly dispersed nickel-modified molybdenum disulfide. The material has good thermal stability and large specific surface area, and has potential applications in the fields of catalysis and electrode materials.

Description

Technical field [0001] The present invention belongs to the technical field of organic synthesis, particularly relates to a method for preparing a highly dispersed nickel-molybdenum disulfide modified. Background technique [0002] Molybdenum disulfide as an important class of material is a two-dimensional planar material has been widely used in catalysis, electrochemistry, electronics devices. In order to enhance the catalytic properties of molybdenum disulfide, except that chemical or mechanical stripping technology, the bulk material is molybdenum disulfide peeling becomes single or multi nanosheet to expose more of the active edge structure by introducing a cation the method makes the material appear more defective bit, while introducing more bimetallic clusters important sulfur-modified molybdenum disulfide is a class method. MMoS industry x (M = Ni, Cu) catalyst as a hydrogenation catalyst is important to study the method of preparing the modified has been an important rese...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/06C23C18/34
Inventor 王峰张超锋高著衍
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI