A nitrogen-doped molybdenum disulfide/c/carbon nanotube composite material

A technology for acidifying carbon nanotubes and molybdenum disulfide, which is applied in the direction of carbon nanotubes, nanocarbons, secondary batteries, etc., can solve problems such as difficulty in obtaining raw materials, complicated and time-consuming operations, loss of nitrogen-doped precursors, etc., and achieve stability Good, simplified production process, fast heating effect

Active Publication Date: 2021-03-02
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0007] In order to solve the problems in the preparation of nitrogen-doped molybdenum disulfide / C / carbon nanotube composite materials in the prior art, the equipment is complicated, the process is cumbersome, the operation is complicated and time-consuming, the product utilization rate is low, the raw material is difficult to obtain, and the nitrogen doping process in the nitrogen doping process is difficult. Due to the low nitrogen doping content caused by the large loss of precursors and the aggregation and accumulation of nanoparticles during the long-term heat treatment process of active components and carbon nanotubes, the present invention provides an efficient, fast, and large-scale synthesis of high nitrogen content doped carbon dioxide The method of molybdenum sulfide / C / carbon nanotube composite material has a high nitrogen content, and the utilization rate of raw materials is significantly improved. The product does not need washing, separation, drying and other processes, and can be directly used as a negative electrode material for lithium batteries, with good application performance

Method used

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  • A nitrogen-doped molybdenum disulfide/c/carbon nanotube composite material
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preparation example Construction

[0040] Preparation of acidified carbon nanotubes: put 1g of carbon nanotubes and 200mL of concentrated sulfuric acid into a three-necked flask, ultrasonically disperse evenly, slowly add 60mL of 70% concentrated nitric acid dropwise, reflux and stir at 60°C for 1h, cool naturally to room temperature, add Dilute with a large amount of deionized water, let it stand for stratification, remove the supernatant, and dialyze the black precipitate at the bottom with deionized water to replace the small molecules in it, so that the surface can be balanced, and a long-term stable and uniform dispersion of carbon nanotubes can be obtained. liquid. The carbon nanotube aqueous dispersion is freeze-dried to obtain acidified carbon nanotube powder, which is placed in a desiccator for subsequent use. Its SEM picture is as follows figure 1 As shown, the structure of one-dimensional carbon nanotubes can be clearly seen, and the walls of carbon nanotubes after acidification treatment are relati...

Embodiment 1

[0043] (1) Weigh 1.0 g of acidified carbon nanotubes and disperse them in 20 mL of 37% formaldehyde aqueous solution, place them in an ultrasonic instrument and disperse evenly, and record them as dispersion liquid A.

[0044] (2) Take 0.5g ammonium paramolybdate and 20mL concentrated ammonia water (NH 3 ·H 2 O) Mix, heat up, add 3.0g ammonium sulfide ((NH 4 ) 2 S), reacted for 0.5 h under the state of magnetic stirring, and then respectively added 0.1 g of tetramethylammonium bromide and 0.6 g of melamine to the solution, and ultrasonically mixed them uniformly to obtain dispersion B.

[0045] (3) Mix Dispersion A and Dispersion B, raise the temperature of the water bath to 60°C and stir for 10 minutes. Then triethanolamine was added to the reaction solution to adjust the pH value of the reaction solution system to 8.0, and the mixture was uniformly mixed by ultrasonic, then the reaction solution was poured into a high-pressure reactor, and the temperature was raised to 12...

Embodiment 2

[0048] (1) Weigh 1.0 g of acidified carbon nanotubes and disperse them in 20 mL of 37% formaldehyde aqueous solution, place them in an ultrasonic instrument and disperse evenly, and record them as dispersion liquid A.

[0049] (2) Take 0.5g ammonium paramolybdate and 20mL concentrated ammonia water (NH 3 ·H 2 O) Mix, heat up, add 9.0g ammonium sulfide ((NH 4 ) 2 S), reacting for 1 h under magnetic stirring, then adding 2.0 g of tetramethylammonium bromide and 2.0 g of melamine to the solution, and ultrasonically mixing to obtain a dispersion B.

[0050] (3) Mix Dispersion A and Dispersion B, raise the temperature of the water bath to 60°C and stir for 10 minutes. Then triethanolamine was added to the reaction solution to adjust the pH value of the reaction solution system to 8.0, and the mixture was uniformly mixed by ultrasonic, then the reaction solution was poured into a high-pressure reactor, and the temperature was raised to 120° C. for 12 hours to react. Filtration a...

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Abstract

The invention discloses a nitrogen-doped molybdenum disulfide / C / carbon nanotube composite material. The preparation method comprises the following steps: taking formaldehyde as a bridge, and carryingout moderate crosslinking on formaldehyde and melamine to form a nitrogen-doped precursor; carrying out hydrothermal reaction to make the nitrogen-doped precursor, an active component precursor and carbon nanotubes interact and uniformly fused; and carrying out solvent-free microwave reaction to synthesize the high-nitrogen-content-doped molybdenum disulfide / C / carbon nanotube composite material. In the preparation process of the composite material, loss caused by sublimation of the nitrogen-doped precursor in the heating process in the traditional nitrogen doping process is avoided, the nitrogen doping efficiency is improved, the reaction conditions are progressively increased from mild to intense, and uniform fusion of the nitrogen-doped precursor, the active component precursor and the carbon nanotubes through interaction is realized. The prepared nitrogen-doped molybdenum disulfide / C / carbon nanotube composite material is good in stability, not prone to denaturation in air, easy to store and large in specific surface area, a good channel is provided for lithium ion transmission when the nitrogen-doped molybdenum disulfide / C / carbon nanotube composite material is used as a lithiumion battery negative electrode material, and large specific capacity and good cycling stability are shown.

Description

technical field [0001] The invention relates to a nitrogen-doped molybdenum disulfide / C / carbon nanotube composite material, in particular to a high-nitrogen-doped molybdenum disulfide / C / carbon nanotube lithium battery negative electrode material, and provides a preparation method thereof, The invention belongs to the technical field of nano composite material and its application. Background technique [0002] Carbon nanotubes are hollow cylinders formed by curling graphite layers, and its bonding method is mainly deformed Sp2 orbitals. When the graphite layer is rolled into carbon nanotubes, the Sp2 hybridization will be partially deformed, so Sp2 tends to form re-hybridization with Sp3. This re-hybridization structure and two-orbital confinement characteristics can endow carbon nanotubes with excellent mechanical, thermal, and thermal properties. Electrical, optical, magnetic and chemical properties. Therefore, carbon nanotubes have higher mechanical strength, better elec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/583H01M4/62H01M10/0525C01B32/158
CPCC01B32/158H01M4/362H01M4/5815H01M4/583H01M4/625H01M10/0525Y02E60/10
Inventor 郭金廖莎张会成王少军凌凤香
Owner CHINA PETROLEUM & CHEM CORP
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