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Electrochemical method for preparing high-purity molybdenum disulfide nanosheet from molybdenite

A molybdenum disulfide and molybdenite technology, which is applied in the field of metallurgical engineering, can solve the problems of high ore raw material grade requirements, complex process, and unguaranteed performance.

Active Publication Date: 2021-06-04
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method also has disadvantages such as low conversion rate, high grade requirements for ore raw materials, complicated process, large pollution, and high cost.
In addition, it is difficult to effectively control the structure and morphology of molybdenum disulfide products using the above two methods, resulting in their performance not being guaranteed
[0003] In recent years, researchers have proposed a variety of nano-MoS 2 Preparation methods, including chemical vapor deposition (CVD), hydrothermal method, organic-inorganic hybrid conversion method, etc. Although the above methods have their own advantages, there is still a long way to go before their large-scale industrial application

Method used

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  • Electrochemical method for preparing high-purity molybdenum disulfide nanosheet from molybdenite
  • Electrochemical method for preparing high-purity molybdenum disulfide nanosheet from molybdenite
  • Electrochemical method for preparing high-purity molybdenum disulfide nanosheet from molybdenite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) the mixture of the NaCl-KCl (50:50mol%) of 1000g is filled in the nickel container of suitable size, then one end of a molybdenum rod is connected with the nickel container, and the other end is stretched out outside the reactor and connected with Connect to the cathode of the external power supply. The nickel container is slowly heated to 800°C in an electric furnace under the protection of an argon atmosphere (the heating rate does not exceed 20°C / min) to melt the chloride salt, and then reduce the temperature of the molten salt to 700°C within 30 minutes.

[0036] (2) The molybdenite ore with a molybdenum content of about 46.33% is mechanically crushed, and screened to obtain molybdenite particles with a particle size below 20mm; select a cylindrical graphite anode, and screen the obtained molybdenite particles (mass about 10g) Put it into a nickel container, and carry out constant voltage electrolysis (electrolyzer voltage: 2.9V) under an argon atmosphere, and t...

Embodiment 2

[0040] (1) Fill the mixture of 700g of NaCl-KCl (45:55mol%) into a nickel container of suitable size, then connect one end of a nickel rod with the nickel container, and the other end stretches out of the reactor And connected to the cathode of the external power supply. The nickel container was slowly heated to 800°C in an electric furnace under the protection of an argon atmosphere to melt the chloride salt, and then the temperature of the molten salt was adjusted to 685°C within 40 minutes.

[0041] (2) The molybdenite ore with a molybdenum content of about 41.57% is mechanically crushed and screened to obtain molybdenite particles with a particle size of 5 to 20 mm; select a flat stainless steel-based molybdenum disulfide coated anode (size is 5 × 5cm 2 ), put the screened molybdenite particles into a nickel container, and perform constant voltage electrolysis (electrolyzer voltage: 2.6V) under an argon atmosphere, and the electrolysis time is 5.0h.

[0042] (3) After the...

Embodiment 3

[0044] (1) The NaCl of 800g is filled in the nickel container of suitable size, then one end of a nickel-chromium alloy rod is connected with the nickel container, and the other end stretches out of the reactor and is connected with the cathode of the external power supply. The nickel container was slowly heated to 850°C in an electric furnace under the protection of an argon atmosphere to melt NaCl.

[0045] (2) Mechanically crush the molybdenite ore with a molybdenum content of about 35%, and screen to obtain molybdenite particles with a particle size below 10 mm; select a cylindrical graphite anode, and put the screened molybdenite particles into a nickel container , Constant current electrolysis (current density of 1500mA / 1g molybdenite) was carried out under an argon atmosphere.

[0046] (3) After the electrolysis, the anode deposition product was collected, washed and dried to obtain molybdenum disulfide nanosheet powder with a purity of about 99.2% (the mass fraction of...

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Abstract

The invention discloses an electrochemical method for preparing a high-purity molybdenum disulfide nanosheet from molybdenite. The purity of the obtained molybdenum disulfide nanosheet reaches 99.0% or above, and the average thickness of the nanosheet is only 10-30 nm. The method comprises the following preparation steps: (1) putting alkali metal chlorate into a nickel reaction container, melting at high temperature, and then reducing the temperature of molten salt to a reaction temperature; (2) adding molybdenite into a nickel container and immersing themolybdenite in molten salt by taking the nickel container as a cathode and the molten salt as electrolyte, and mounting an anode for electrolysis; and (3) after the electrolysis is finished, taking out the anode, cooling to room temperature in an inert atmosphere, collecting anode surface sediments, and washing and drying to obtain the high-purity molybdenum disulfide powder. The method is simple to operate, clean in process and low in preparation cost; and the obtained molybdenum disulfide nanosheet is stable in property, and shows relatively high lithium storage performance and electrochemical stability when being used as a lithium ion battery negative electrode material.

Description

technical field [0001] The invention belongs to the technical field of metallurgical engineering, and specifically relates to an electrochemical method for preparing high-purity molybdenum disulfide nanosheets in a short process using molybdenite as a raw material, and the application of the molybdenum disulfide material in the field of lithium batteries. Background technique [0002] Molybdenum disulfide nanomaterials show broad application prospects in the fields of optoelectronic device manufacturing, heterogeneous photocatalysis, solid-state lubricant materials, and electrochemical energy storage due to their special chemical and electronic structures and excellent mechanical, optical, and electrical properties. However, the large-scale preparation of high-performance nanomolybdenum disulfide still faces many problems. At present, molybdenite (mainly composed of MoS) is mostly used in industry 2 , is the most important source of molybdenum for the preparation of molybde...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/01H01M4/58H01M10/0525B82Y40/00
CPCC25B1/00H01M4/5815H01M10/0525B82Y40/00H01M2004/027Y02E60/10
Inventor 汪的华蒋睿赵笑宇邓艺菲胡良友
Owner WUHAN UNIV
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