Preparation method of bamboo-like nitrogen-doped carbon nanotubes loaded with metal monoatoms and nanoparticles

A nanoparticle and metal-loaded technology, which is applied in chemical instruments and methods, catalyst activation/preparation, organic chemistry, etc., can solve the problems of highly toxic cyanide and cumbersome preparation process, and achieve high reaction yield and simple process , low cost effect

Active Publication Date: 2021-12-14
HEBEI UNIV OF TECH
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Problems solved by technology

[0004] Although there have been a few reports of ZIF-derived bamboo-shaped nanotubes, the preparation process is cumbersome, and a large amount of organic solvents are needed in the preparation process. Dicyandiamide and melamine need to be added in the pyrolysis process. It is easy to form highly toxic cyanide when it is decomposed (Small 2020, 16(41), 2002124)

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  • Preparation method of bamboo-like nitrogen-doped carbon nanotubes loaded with metal monoatoms and nanoparticles
  • Preparation method of bamboo-like nitrogen-doped carbon nanotubes loaded with metal monoatoms and nanoparticles
  • Preparation method of bamboo-like nitrogen-doped carbon nanotubes loaded with metal monoatoms and nanoparticles

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[0029] The preparation process of the present invention is as follows, (1) using 2-methylimidazole, metal salts, and zinc-containing compounds as precursors, preparing a mixture containing ZIFs single crystals by ball milling, (2) obtaining supported metal single atoms by high temperature pyrolysis and nanoparticle bamboo-like nitrogen-doped carbon nanotubes.

[0030] The preparation process of the present invention is simple, easy to prepare on a large scale, and the obtained product has excellent photothermal conversion performance and highly active multifunctional sites, and bamboo-shaped nanotubes are easy to expose more internal active sites and improve mass transfer efficiency; metal single atoms And nanoparticles are beneficial to increase the ability of synergistic catalysis. These characteristics make it have great potential application value in the fields of micro-nano reactor and synergistic catalysis.

[0031] Among them, the metal salt Ni(NO 3 ) 2 ·6H 2 O, Ni(N...

Embodiment 1

[0033] (1) Add 28mmol of 2-methylimidazole, 1mmol of Ni(NO 3 ) 2 ·6H 2 0, 5mmol of zinc oxide (the total amount of reactants is 3.0g) and 10 grinding balls (diameter 0.5cm), ball milled for 3h under the condition of 1000r / min at the ball milling jar speed, to obtain a mixture containing ZIFs single crystal.

[0034] figure 1 It is an SEM photo obtained by scanning the mixture containing ZIFs single crystal with a FEI Nano SEM 450 scanning electron microscope. It can be seen from the figure that the single crystal ZIF presents a rhombic dodecahedral structure with a particle size of 200-1000nm.

[0035] (2) Place the resulting mixture containing ZIFs single crystals in a quartz boat, and heat it in a tube furnace at 5°C min -1 Raise from room temperature to 1000° C. for 3 hours, and cool down to room temperature naturally to obtain metal single atoms and nanoparticle bamboo-shaped nitrogen-doped carbon nanotubes.

[0036] figure 2 and image 3 The SEM and STEM photos ob...

Embodiment 2

[0043] (1) Add 28mmol of 2-methylimidazole, 1mmol of Ni(NO 3 ) 2 ·6H 2 0, 5mmol of zinc hydroxide (the total amount of reactants is 3.1g) and 10 grinding balls (diameter 0.5cm), ball milling for 3h at a rotating speed of 800r / min to obtain a mixture containing ZIFs single crystal.

[0044] (2) Place the resulting mixture containing ZIFs single crystals in a quartz boat, and heat it in a tube furnace at 5°C min -1 Raise from room temperature to 1100° C. for 2 hours, and cool down to room temperature naturally to obtain supported metal single atoms and nanoparticle bamboo-shaped nitrogen-doped carbon nanotubes.

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Abstract

The invention relates to a preparation method of bamboo-like nitrogen-doped carbon nanotubes loaded with metal monoatoms and nanoparticles. The method comprises the following steps of: adding 2-methylimidazole, metal salt, a zinc-containing compound and grinding balls into a ball milling tank, and carrying out ball milling for 2-8 hours to obtain a mixture containing ZIFs single crystals; and placing the mixture containing ZIFs single crystals in a quartz boat, heating the mixture to 800-1100 DEG C from room temperature at a speed of 2-5 DEG C min <-1 > in a tubular furnace, maintaining the temperature for 1-3 hours, and naturally cooling to room temperature to finally obtain bamboo-like nitrogen-doped carbon nanotubes loaded with metal monoatoms and nanoparticles. The steps of washing, separating and the like are not needed, the method has huge potential application value in the fields of photo-thermal catalysis, concerted catalysis and the like, and the application range of the method in the catalysis field is widened.

Description

technical field [0001] The invention relates to the technical field of carbon nanotube one-dimensional composite material preparation, in particular to a method for preparing metal single atoms and nano-particle bamboo-shaped nitrogen-doped carbon nanotubes. Background technique [0002] Due to their excellent mechanical, electrical and chemical properties, carbon nanotubes are widely used in energy storage and conversion, catalytic conversion, lithium-ion batteries, sensors and other fields (Energy Storage Materials 2021, 43, 365-374). However, pure carbon nanotubes have fewer active sites, which limits the application of carbon nanotubes in the field of catalysis. In order to improve the surface chemical properties of carbon nanotubes and enhance their catalytic performance, nitrogen doping or supporting metal nanoparticles and single atoms is an effective and feasible method. Nitrogen-doped carbon nanotubes containing metal single atoms have attracted extensive attention...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/00B01J37/08C07D317/36
CPCB01J27/24B01J35/004B01J37/086B01J37/0036C07D317/36Y02E60/50
Inventor 张旭郭迎春王小梅
Owner HEBEI UNIV OF TECH
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