Highly dispersed palladium/carbon nanometer tube catalyst for anthraquinone hydrogenation and preparation method thereof

A technology of carbon nanotubes and catalysts, which is applied in the field of highly dispersed palladium/carbon nanotube catalysts and its preparation, can solve the problems of unsatisfactory reduction effect of palladium active components, insignificant catalyst effect, and small amount of reducing agent, etc., to achieve improved Effective utilization rate, improved hydrogenation efficiency, and easy recovery of palladium

Active Publication Date: 2013-04-24
XIAMEN UNIV +2
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  • Summary
  • Abstract
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Problems solved by technology

Although carbon nanotubes are used as the carrier and palladium nanoparticles as the active component, the reduction effect of the palladium active component is not ideal due to the high concentration of Pd, the small amount of reducing agent, and the short reduction time. It shows certain activity during the hydrogen reduction process, but the catalyst prepared by repeating this method has no obvious effect in the anthraquinone hydrogenation system

Method used

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  • Highly dispersed palladium/carbon nanometer tube catalyst for anthraquinone hydrogenation and preparation method thereof
  • Highly dispersed palladium/carbon nanometer tube catalyst for anthraquinone hydrogenation and preparation method thereof
  • Highly dispersed palladium/carbon nanometer tube catalyst for anthraquinone hydrogenation and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0062] In the slurry bed of the reaction vessel, add carbon nanotubes and water according to the mass ratio of CNTs (carbon nanotubes): water = 1:45, stir mechanically and ultrasonically until the carbon nanotubes are uniformly dispersed, and prepare a carbon nanotube suspension. After 20 minutes, keep mechanical and ultrasonic stirring, slowly add palladium chloride hydrochloric acid with an appropriate concentration of 0.25g / L to the carbon nanotube suspension according to the loading of Pd (nano-palladium particles) being 0.28wt% of the carbon nanotubes Solution, obtain palladium ion / carbon nanotube suspension, after 20 minutes, add the NaOH alkaline solution of 15wt% to adjust the pH of palladium ion / carbon nanotube suspension to be 9~12, continue to keep mechanical and ultrasonic stirring, be warming up to 40 ℃ and add excess formaldehyde solution, and continue to adjust with NaOH solution and keep the pH at 10~14 until the pH is basically unchanged within 30min, filter, w...

Embodiment 2

[0072] In the slurry bed of the reaction vessel, add carbon nanotubes and water according to the mass ratio of CNTs (carbon nanotubes): water = 1:45, stir mechanically and ultrasonically until the carbon nanotubes are uniformly dispersed, and prepare a carbon nanotube suspension. After 22 minutes, keep mechanical and ultrasonic stirring, slowly add palladium chloride hydrochloric acid with an appropriate concentration of 0.50g / L to the carbon nanotube suspension according to the loading of Pd (nano-palladium particles) being 0.84wt% of the carbon nanotubes Solution, obtain palladium ion / carbon nanotube suspension, after 15 minutes, add the NaOH alkaline solution of 15wt% to adjust the pH of palladium ion / carbon nanotube suspension to be 9~12, keep mechanical and ultrasonic stirring, be warming up to 40 ℃ and add excess formaldehyde solution, and continue to adjust with NaOH solution and keep the pH at 10~14 until the pH is basically unchanged within 30min, filter, wash, and...

Embodiment 3

[0074] In the slurry bed of the reaction vessel, add carbon nanotubes and water according to the mass ratio of CNTs (carbon nanotubes): water = 1:45, stir mechanically and ultrasonically until the carbon nanotubes are uniformly dispersed, and prepare a carbon nanotube suspension. After 26 minutes, keep mechanical and ultrasonic stirring, slowly add palladium chloride hydrochloric acid with an appropriate concentration of 1.0g / L to the carbon nanotube suspension according to the loading of Pd (nano-palladium particles) at 2.52wt% of the carbon nanotubes Solution, obtain palladium ion / carbon nanotube suspension, after 18 minutes, add the NaOH alkaline solution of 15wt% to adjust the pH of palladium ion / carbon nanotube suspension to be 10~11, continue to keep mechanical and ultrasonic stirring, be warming up to 40 ℃ and add excess formaldehyde solution, and continue to use NaOH solution to adjust and keep the pH at 12~14 until the pH is basically unchanged within 30min, filter...

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Abstract

The invention discloses a highly dispersed palladium/carbon nanometer tube catalyst for anthraquinone hydrogenation and a preparation method thereof, and relates to a catalyst and a preparation method. According to the invention, a carbon nanometer tube industrial product with good conductivity, heat conductivity, high mechanical strength and huge external specific surface is used as a palladium carrier; simultaneously ultrasonic is utilized to further enhance the dispersity and uniformity of palladium and the carbon nanometer tube; and a nanometer palladium catalyst uniformly loaded on the surface of the carbon nanometer tube is prepared in a slurry reactor by adopting a liquid phase reduction method. The catalyst needs no extrusion molding and can be directly suspended in the liquid phase for normal-pressure or pressurized hydrogenation of anthraquinone; the activity of the catalyst is not reduced after the catalyst is used for a plurality of times by filtration and separation; moisture, acid and alkaline do not influence the use effect; the catalytic activity of the new catalyst is 4-8 times higher than that of the traditional Pd/gamma-Al2O3 catalyst, and the amount of the catalyst used can be greatly reduced. The catalyst can be used for replacing the traditional catalyst, the post treatment of the traditional catalyst is simplified, the treatment capability of a device is greatly increased, and the operation cost is lowered.

Description

technical field [0001] The invention relates to a catalyst and a preparation method, in particular to a highly dispersed palladium / carbon nanotube catalyst and a preparation method for anthraquinone hydrogenation. Background technique [0002] Hydrogen peroxide is a green chemical product widely used in chemical industry, paper making, environmental protection, electronics, food, medicine, textile, mining, agricultural waste processing and other industries. At present, there are many production methods for hydrogen peroxide, among which the anthraquinone method is the most important method for producing hydrogen peroxide at home and abroad, accounting for more than 95% of the total industrial production capacity. Anthraquinone hydrogenation is the core of the anthraquinone process. Supported palladium catalyst is currently the most effective and widely used catalyst for hydrogenation of anthraquinone. At present, Pd / γ-Al is widely used in industry 2 o 3 Catalyst, but its ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C01B15/023
Inventor 李大川吕明超李菲菲尹应武廖能成覃秀凤韦杰陈韡韦岸鑫
Owner XIAMEN UNIV
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