Size-adjustable palladium-based catalyst limited by carbon nanotubes as well as preparation method and application of size-adjustable palladium-based catalyst

A carbon nanotube and catalyst technology, which is applied in the field of size-adjustable palladium-based catalyst and its preparation, can solve the problems of lack of metal nanoclusters or metal single atoms, intercalation, etc., and achieves the improvement of atom utilization efficiency, and the method is simple and easy to implement. The effect of large reaction residence time

Active Publication Date: 2020-09-15
ZHUHAI FUDAN INNOVATION INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, limited by traditional preparation methods, there is no effective means to embed metal nanoclusters or metal single atoms into the confinement space of carbon nanotubes with a spatial scale of nanometer scale.

Method used

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  • Size-adjustable palladium-based catalyst limited by carbon nanotubes as well as preparation method and application of size-adjustable palladium-based catalyst
  • Size-adjustable palladium-based catalyst limited by carbon nanotubes as well as preparation method and application of size-adjustable palladium-based catalyst
  • Size-adjustable palladium-based catalyst limited by carbon nanotubes as well as preparation method and application of size-adjustable palladium-based catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) 2 g of carbon nanotubes were placed in a mixed solution of 120 mL of concentrated sulfuric acid and 40 mL of concentrated nitric acid, and heated and acidified at 60 °C for 3 hours. Then suction filtration washing and dialysis until the pH of the dispersion is close to neutral;

[0029] (2) Take 100 mL of the carbon nanotube dispersion with a concentration of 1 mg / mL in a beaker, add 121 mg of tris (Tris) and 200 mg of dopamine hydrochloride, and keep stirring for 12 hours to make the dopamine hydrochloride Polydopamine is polymerized to form polydopamine and wrapped on carbon nanotubes to obtain CNT@PDA composite materials;

[0030] (3) The obtained CNT@PDA composite material was annealed at 800 °C for 1 hour under the protection of an inert gas atmosphere, so that the polydopamine PDA component in it was annealed to form nitrogen-doped carbon, and CNT@ NC composite materials;

[0031] (4) Disperse the obtained CNT@NC composite material in deionized water to prep...

Embodiment 2

[0035] (1) 2 g of carbon nanotubes were placed in a mixed solution of 160 mL of concentrated sulfuric acid and 40 mL of concentrated nitric acid, and heated and acidified at 65 °C for 2 hours. Then suction filtration washing and dialysis until the pH of the dispersion is close to neutral;

[0036](2) Take 100 mL of the carbon nanotube dispersion with a concentration of 1 mg / mL in a beaker, add 121 mg of tris (Tris) and 200 mg of dopamine hydrochloride, and keep stirring for 24 hours to make the dopamine hydrochloride Polydopamine is polymerized to form polydopamine and wrapped on carbon nanotubes to obtain CNT@PDA composite materials;

[0037] (3) The obtained CNT@PDA composite material was annealed at 1000 °C for 2 hours under the protection of an inert gas atmosphere, so that the polydopamine PDA component in it was annealed to form nitrogen-doped carbon, and CNT@ NC composite materials;

[0038] (4) Disperse the obtained CNT@NC composite material in deionized water to pre...

Embodiment 3

[0042] (1) 2 g of carbon nanotubes were placed in a mixed solution of 120 mL of concentrated sulfuric acid and 40 mL of concentrated nitric acid, and heated and acidified at 65 °C for 2 hours. Then suction filtration washing and dialysis until the pH of the dispersion is close to neutral;

[0043] (2) Take 100 mL of the carbon nanotube dispersion with a concentration of 2 mg / mL in a beaker, add 242 mg of tris (Tris) and 150 mg of dopamine hydrochloride, and keep stirring for 24 hours to make the dopamine hydrochloride Polydopamine is polymerized to form polydopamine and wrapped on carbon nanotubes to obtain CNT@PDA composite materials;

[0044] (3) The obtained CNT@PDA composite material was annealed at 1000 °C for 2 hours under the protection of an inert gas atmosphere, so that the polydopamine PDA component in it was annealed to form nitrogen-doped carbon, and CNT@ NC composite materials;

[0045] (4) Disperse the obtained CNT@NC composite material in deionized water to pr...

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Abstract

The invention belongs to the technical field of catalysts, and particularly relates to a size-adjustable palladium-based catalyst limited by carbon nanotubes as well as a preparation method and an application of the size-adjustable palladium-based catalyst. By improving the whole process flow and the reaction conditions and parameters (such as types and proportions of reaction raw materials, reactant concentration and reaction temperature) of all key process steps, precious metal active substances are limited in the inner cavity of the carbon nano tube, and the metal size can be regulated andcontrolled by controlling the reaction conditions. The preparation method is simple in process, convenient to operate, cheap and easily available in reaction materials, and capable of preparing the confinement catalyst with specific catalytic performance according to specific requirements, including a carbon nano tube confinement palladium monatomic catalyst and a carbon nano tube confinement palladium cluster catalyst, so that accurate regulation and control between the loading capacity and the size are realized. The prepared palladium-based catalyst can be used for catalyzing a reduction reaction of an aromatic nitro compound and shows excellent catalytic activity.

Description

technical field [0001] The invention belongs to the technical field of catalysts, in particular to a size-adjustable palladium-based catalyst confined by carbon nanotubes and its preparation method and application. Background technique [0002] Supported noble metal-based (such as Pd, Pt) catalysts have been widely used in many fields such as industrial catalysis and chemical synthesis, and the preparation of catalysts with high catalytic activity and low price is still the main development direction of the catalytic industry. At present, most supported catalysts use metal nanoparticles as active centers. Metal nanoparticles or cluster catalysts have good apparent catalytic activity, but their atom utilization is low and their manufacturing costs are high, making them unsuitable for large-scale applications. In addition, metal single-atom catalysts are very easy to agglomerate into nanoparticles due to their high surface energy, which is difficult to exist stably. In many ...

Claims

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Application Information

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IPC IPC(8): B01J21/18B01J27/24C07C213/02C07C215/76
CPCB01J27/24B01J21/185C07C213/02B01J35/393C07C215/76
Inventor 王帅池凯奚江波
Owner ZHUHAI FUDAN INNOVATION INST
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