Method for preparing load-type noble metal nanometer catalyst by solvent-free microwave-assisted pyrolysis method

A microwave-assisted, precious metal technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve problems such as cumbersome steps, high cost of solvents, and unfavorable industrialization , to achieve the effects of reduced dosage, environmental friendliness, and good industrial application prospects

Inactive Publication Date: 2011-04-27
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the steps are cumbersome a...

Method used

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  • Method for preparing load-type noble metal nanometer catalyst by solvent-free microwave-assisted pyrolysis method
  • Method for preparing load-type noble metal nanometer catalyst by solvent-free microwave-assisted pyrolysis method
  • Method for preparing load-type noble metal nanometer catalyst by solvent-free microwave-assisted pyrolysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 0.0316g triruthenium dodecacarbonyl (Ru: 15wt.%) and 0.1g untreated carbon nanotubes, mix them, grind them in an agate mortar for 20min, and put them into a fluidized reaction tube, purging with argon 2h, microwave 800W heating 1min, 3min, 5min, 7min, 15min respectively, the argon flow rate in the reaction is: 100mL / min, cool to room temperature in the argon atmosphere, about 12h, can get the carbon nanotube supported ruthenium catalyst (Ru / CNTs).

[0020] Sample serial number

Embodiment 2

[0022] Weigh 0.0316g (15wt.%), 0.0210g (10wt.%), 0.0105g (5wt.%) triruthenium dodecacarbonyl and 0.1g untreated carbon nanotubes respectively, mix and grind in an agate mortar After 20 minutes, put it into a fluidized reaction tube, purge it with argon for 2 hours, and heat it with a microwave at 800W for 5 minutes. Supported ruthenium catalysts (Ru / CNTs). The XRD spectrum of the obtained Ru / CNTs is as follows figure 2 shown. It was identified as metal ruthenium by X-ray powder diffraction. The transmission electron micrographs of the obtained samples are shown in figure 1 , 2 , 3.

[0023] Sample serial number

Embodiment 3

[0025] Measure 60mL of deionized water, then measure 60mL of concentrated nitric acid, add the concentrated nitric acid into the water and stir. Measure 180mL of concentrated sulfuric acid, make the volume ratio of concentrated sulfuric acid, concentrated nitric acid and water 3:1:1, and mix the three evenly. Weigh 3 g of carbon nanotubes and add them into the mixed acid. After ultrasonication for 5 min, reflux at 120° C. and keep the temperature constant for 4 h. Cool to room temperature, filter and wash to pH = 6, dry at 120°C for 3 hours, and store for future use.

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Abstract

The invention discloses a method for preparing a load-type noble metal nanometer catalyst by a solvent-free microwave-assisted pyrolysis method and application thereof, belonging to the technical field of catalysis. The method comprises the following steps of: fully grinding and mixing a noble metal coordination compound and a vector, and forming the stable load-type noble metal catalyst by the microwave-assisted pyrolysis in an inert atmosphere. The invention has the advantages of simple process, no solvent, low energy consumption in the process, and the like. In the prepared catalyst, Ru, Rh, Re, Pd, Pt, and other particles are evenly distributed on the outer surface of the vector, therefore, the utilization ratio of noble metal particles is improved, the cost of the catalyst is effectively reduced, and the method has potential industrial application value. The load-type noble metal catalyst has favorable catalysis performance in a plurality field of hydrogenation, hydrogenolysis, ammonia synthesis, ammonia decomposition, hydrocarbon synthesis, hydrogenation formylation, and the like, shows the characteristics of high activity, good stability, reduced reaction energy consumption, and the like and has wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalysis, and relates to a method for preparing a loaded noble metal nano-catalyst material, in particular to a method for decomposing noble metal complexes into noble metals by using a solvent-free microwave-assisted pyrolysis method, and using the prepared catalyst for Catalytic reactions such as selective hydrogenation of alkenals, synthesis of ammonia and decomposition of ammonia. Background technique [0002] Supported noble metal catalysts have good catalytic performance in many fields such as hydrogenation, hydrogenolysis, ammonia synthesis, hydrocarbon synthesis, hydroformylation, etc., and have the characteristics of high activity, good stability, and reduced reaction energy consumption. application prospects. The use of the carrier is beneficial to improve the dispersion of metals, especially to reduce the amount of precious metals, improve its activity, reduce the cost of the ca...

Claims

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Application Information

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IPC IPC(8): B01J37/34B01J23/46C07C27/04C07C47/228C07C45/62C07C33/32C07C29/141
Inventor 梁长海倪晓娟
Owner DALIAN UNIV OF TECH
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