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Preparation method of nickel nanoparticles-loaded multi-wall carbon nanotube catalytic agent

A multi-walled carbon nanotube, nickel nanoparticle technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of agglomeration, uneven loading, and it is difficult to control the reaction rate of nickel particles Growth environment and other problems, to achieve the effect of fine particle size

Inactive Publication Date: 2011-08-31
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, the process of preparing nickel-supported multi-walled carbon nanotube catalysts by liquid-phase chemical reduction method has the following problems: 1) The surface of carbon nanotubes is inert, and acidification conditions will affect the degree of introduction of surface functional groups. Also be difficult to make the uniform loading of nickel particle; 2) direct liquid phase chemical reduction method is difficult to control the rate of reaction and the environment that nickel particle grows, the nickel particle particle size in the prepared catalyst is too large and agglomeration phenomenon is serious; 3) nickel The uneven loading of particles on the surface of carbon nanotubes results in a small specific surface area and inhibits their electrocatalytic performance

Method used

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  • Preparation method of nickel nanoparticles-loaded multi-wall carbon nanotube catalytic agent
  • Preparation method of nickel nanoparticles-loaded multi-wall carbon nanotube catalytic agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Carbon tube pretreatment:

[0023] (a) Acidification: Disperse 2g of multi-walled carbon nanotubes in 120ml of mixed acid solution, the volume ratio of concentrated nitric acid (65%): concentrated sulfuric acid (98%)=1:3, reflux at 60°C for 5h, wash with deionized water until Neutral, vacuum dried for 12h.

[0024] (b) Sensitization: Ultrasonic dispersion (40kHz) of 40mg acidified carbon tubes in 40ml containing 0.08g SnCl 2 , 0.1ml 1mol / L HCl and 0.01g PDMA aqueous solution for 30min, filtered, washed with deionized water, and dried in vacuum for 1h.

[0025] (c) Activation: ultrasonically disperse 40mg of sensitized carbon nanotubes in 40ml containing 0.0084g PdCl 2 , 0.48ml1mol / L HCl, 0.01g PDMA aqueous solution for 30min, thoroughly washed with deionized water, and vacuum dried for 24h.

[0026]2) Mix 50 mg of treated multi-walled carbon nanotubes in 50 ml of aqueous solution, add 0.101 g of NiCl according to 50 wt % nickel loading 2 ·6H 2 O, and 0.182g (10m...

Embodiment 2

[0030] 1) Carbon tube pretreatment:

[0031] (a) Acidification: Disperse 3g of multi-walled carbon nanotubes in 120ml of mixed acid solution, the volume ratio of concentrated nitric acid (65%): concentrated sulfuric acid (98%)=1:3. Condensate and reflux at 80°C for 6h, wash with deionized water until Neutral, vacuum dried for 12h.

[0032] (b) Sensitization: Ultrasonic dispersion (40kHz) of 60mg acidified carbon tubes in 60ml containing 0.12g SnCl 2 , 0.15ml 1mol / L HCl and 0.03g PDMA aqueous solution for 30min, filtered, washed thoroughly with deionized water, and dried in vacuum for 1h.

[0033] (c) Activation: ultrasonically disperse 60mg of sensitized carbon nanotubes in 60ml containing 0.0126g PdCl 2 , 0.72ml 1mol / L HCl, 0.03g PDMA aqueous solution for 30min, rinse thoroughly with deionized water, and vacuum dry for 24h.

[0034] 2) Mix 50 mg of treated multi-walled carbon nanotubes in 50 ml of aqueous solution, add 0.101 g of NiCl according to 50 wt % nickel loading 2...

Embodiment 3

[0038] 1) Carbon tube pretreatment:

[0039] (a) Acidification: Disperse 2g of multi-walled carbon nanotubes in 100ml of mixed acid solution, the volume ratio of concentrated nitric acid (65%): concentrated sulfuric acid (98%)=1:3. Condensate and reflux at 60°C for 8h, wash with deionized water until Neutral, vacuum dried for 12h.

[0040] (b) Sensitization: Ultrasonic dispersion (40kHz) of 40mg acidified carbon tubes in 20ml containing 0.04g SnCl 2 , 0.05ml 1mol / L HCl and 0.005g PDMA aqueous solution for 30min, filtered, washed thoroughly with deionized water, and dried in vacuum for 1h.

[0041] (c) Activation: ultrasonically disperse 40mg of sensitized carbon nanotubes in 20ml containing 0.0042g PdCl 2 , 0.24ml1mol / L HCl, and 0.005g PDMA aqueous solution for 30min; thoroughly wash, vacuum dry for 24h, thoroughly wash with deionized water, and vacuum dry for 24h.

[0042] 2) Mix 50 mg of treated multi-walled carbon nanotubes in 50 ml of aqueous solution, add 0.101 g of Ni...

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Abstract

The invention discloses a preparation method of a nickel nanoparticles-loaded multi-wall carbon nanotubes catalytic agent, belonging to the technical field of energy material. The preparation method comprises the steps of acidifying multi-wall carbon nanotubes (MWCNTs) in mixed acid, leading in functional groups, respectively sensitizing and activating the MWCNTs in hydrochloric acid water solution of SnCl2 and PdCl2 to lead in a Pd active site, ultrasonically dispersing nickel salt NiCl2.6H2O and the pretreated MWCNTs in the water solution according to a certain proportion, adding a certain quantity of cetyl trimethyl ammonium bromide (CTAB) to be taken as a complexing agent, complexing Ni2+and an added reducing agent to control the velocity and the steps of the reaction, adjusting a PH value to be a required value, and adding the reducing agent within the time required by the reaction at a certain temperature. The method obtains the nickel nanoparticles which are even in distribution and fine in grain diameters on the surfaces of multi-wall carbon nanotubes.

Description

technical field [0001] The invention belongs to the technical field of energy materials, and in particular relates to a liquid-phase chemical reduction preparation method of a nickel nanoparticle-loaded multi-walled carbon nanotube catalyst applied to an ethanol fuel cell. Background technique [0002] In 1839, the British William Grove first announced the working principle of the fuel cell, creating a new energy conversion technology since then. Fuel cells are the fourth type of power generation technology after hydropower, thermal power and nuclear energy utilization. It can directly convert the chemical reaction free energy change into electrical energy through the electrode-electrolyte system. Compared with traditional conversion methods, fuel cells do not require thermal energy conversion and mechanical energy conversion processes, avoid energy loss and limitations of the Carnot cycle, and significantly improve energy conversion efficiency. Fuel cells not only have hi...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J37/16H01M4/90
CPCY02E60/50
Inventor 王峰刘铮刘景军王建军覃事永张良虎
Owner BEIJING UNIV OF CHEM TECH
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