Electrochemical reducing process for preparing nanometer MOS2 particle

A molybdenum disulfide and nanoparticle technology, applied in the electrolysis process, electrolysis components and other directions, can solve the problems of expensive raw materials, high reaction temperature, large product particle size, etc., to promote promotion and application, good monodispersity, process simple effect

Inactive Publication Date: 2007-06-27
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

The reduction method is not conducive to control because the reaction mostly occurs in a heterogeneous system; the operation and equipment in the preparation process of the decomposition method are relatively simple, and it is widely used at present, but the temperature control in the method is very important. Amorphous MoS2, crystals are easy to grow at a higher temperature, and the elemental sulfur produced at the same time will cause serious corrosion to the equipment; due to the different raw materials used in the oxidation method, the product particle size will be large, the reaction temperature is too high, or the raw material price Disadvantages such as expensive and highly toxic; electrochemical methods mainly focus on the preparation of molybdenum sulfide thin films

Method used

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  • Electrochemical reducing process for preparing nanometer MOS2 particle
  • Electrochemical reducing process for preparing nanometer MOS2 particle

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Embodiment 1

[0026] Take by weighing 12.4g ammonium molybdate tetrahydrate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) Prepare a 100mL 0.1mol / L solution, heat to 50-60°C; then pass in hydrogen sulfide gas, absorb the tail gas with sodium hydroxide solution, and constantly adjust the pH value to 8.0 during the reaction process. After about 6 hours, the color of the solution turned into dark brownish red completely. After the reaction was completed, heating was stopped, and brownish red crystals could be obtained by cooling, which were purified and dried in vacuo.

[0027] Take by weighing 0.025g ammonium tetrathiomolybdate and 0.75g potassium chloride, dissolve in 100mL double-distilled water successively, pass nitrogen to remove dissolved oxygen; Electrode, the standard calomel electrode is the reference electrode, the platinum wire is the counter electrode, the constant current mode is adopted, and the current density is controlled at 2mAcm -2 , the reaction time is 30 minutes. After the reaction,...

Embodiment 2

[0030] The preparation of ammonium tetrathiomolybdate is the same as above.

[0031] Then take by weighing 0.025g ammonium tetrathiomolybdate, 0.75g potassium chloride and 0.273g tetraoctyl ammonium bromide, dissolve in 100mL double-distilled water successively, nitrogen gas removes dissolved oxygen; And in the self-made electrochemical reaction cell Graphite is used as the working electrode, the standard calomel electrode is used as the reference electrode, and platinum wire is used as the counter electrode. The constant current mode is adopted, and the current density is controlled at 2mAcm -2 , the reaction time is 30 minutes. After the reaction, there was black sediment at the bottom of the reaction tank, which was filtered, washed and dried to obtain the target product.

[0032] Figure 3 and Figure 4 are transmission electron microscope photographs of molybdenum disulfide nanoparticles obtained under the condition of the presence of surfactants at different magnification...

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Abstract

The present invention discloses preparation process of nanometer MoS2 particle. Through electrochemical reduction on ammonium tetrathiomolybdate, nanometer MoS2 particle dispersing in organic solvent and with homogeneous size and high monodispersion is prepared. The present invention expands the preparation measures of nanometer MoS2 particle, and the nanometer MoS2 particle may be used widely in petroleum refining for hydrodesulfurizing and hydrodenitrogenation, chemical industry, and other fields.

Description

technical field [0001] The invention relates to an electrochemical reduction preparation method of organic dispersed molybdenum disulfide nanoparticles. Background technique [0002] Transition metal layered binary compounds (MX 2 ) has attracted people's attention because of its good optical, electrical, lubricating, and catalytic properties, and molybdenum disulfide is one of the typical representatives. MoS 2 Belonging to the hexagonal crystal system, it is a compound with antimagnetic and semiconductor properties. It has quite a lot of Mo-S facets, large specific surface area, strong covalent bonds in the layer, and weak van der Waals force between layers. Therefore, it is easy for layers to have good anisotropy and low friction coefficient, and S element has strong adhesion to metal, making MoS 2 It can be well attached to the metal surface and always play a lubricating function, especially under high temperature, high vacuum and other conditions, it still has a low ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/00
Inventor 王晓波刘维民
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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