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Preparation and application of catalyst with metal loaded on inner wall of silicon dioxide nanotube

A technology of silica and supported catalysts, which can be used in metal/metal oxide/metal hydroxide catalysts, preparation of organic compounds, catalysts for physical/chemical processes, etc., and can solve the problems of complex reaction system and low catalytic activity.

Pending Publication Date: 2022-04-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When this catalyst does not add CeO2, the selectivity of cyclohexylmethylamine is only 43%, the catalytic activity is low, and after adding CeO2, the reaction system is complex

Method used

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  • Preparation and application of catalyst with metal loaded on inner wall of silicon dioxide nanotube
  • Preparation and application of catalyst with metal loaded on inner wall of silicon dioxide nanotube
  • Preparation and application of catalyst with metal loaded on inner wall of silicon dioxide nanotube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0016] Preparation of Example 1-3 Ru-CNTs-1(2 or 3)-red

[0017] Ru-CNTs-1-red is prepared by impregnation method, as follows:

[0018] Add 50 mg of multi-walled carbon nanotubes with an outer diameter of 10-20 nm and a length of 5-30 μm into 10 mL of ultrapure water, and ultrasonically disperse the carbon nanotubes in the ultrapure water for 30 minutes. Then the corresponding amount of Ru precursor solution RuCl 3 Added to the aqueous solution of CNTs, stirred for 24h, 60°C vacuum rotary evaporation, then dried in an oven at 110°C for 12h, after grinding fully, in a tube furnace at a volume concentration of 30%H 2 H 2 and N 2 Reduction under mixed gas conditions, the reduction temperature is 250 ° C, the reduction time is 2h, wherein the mass fraction of Ru is 1wt%, 2wt% and 8wt%, respectively, and the catalysts obtained are recorded as Ru-CNTs-1 (2 or 3 )-red.

Embodiment 4

[0019] Example 4 Preparation of Ru-CNTs-4-red

[0020] Add 50 mg of carbon nanotubes with an outer diameter of 10-20 nm and a length of 5-30 μm into 10 mL of acetone, and ultrasonically disperse the carbon nanotubes in the acetone for 30 minutes. Then the corresponding amount of Ru precursor ruthenium acetylacetonate was added to the acetone solution of CNTs, stirred for 24 h, vacuum rotary evaporated at 30 °C, and then dried in an oven at 110 °C for 12 h, and then ground in a tube furnace at a volume concentration of 30%. h 2 H 2 and N 2 Reduction under the condition of mixed gas, the reduction temperature is 250 ℃, the reduction time is 2h, the obtained catalyst is marked as Ru-CNTs-4-red. The mass fraction of Ru is 2wt%, and that of carbon nanotubes is 98wt%.

Embodiment 5

[0021] Example 5 Preparation of Ru-CNTs-5-red

[0022] Add 50 mg of carbon nanotubes with an outer diameter of 10-20 nm and a length of 5-30 μm into 10 mL of isopropanol, and ultrasonically disperse the carbon nanotubes in the isopropanol evenly for 30 minutes. Subsequently, a corresponding amount of Ru precursor hexaamine ruthenium trichloride was added to the isopropanol solution of CNTs, stirred for 24 h, vacuum rotary evaporated at 40 °C, and then dried in an oven at 110 °C for 12 h, and then ground in a tube furnace In volume concentration 30%H 2 H 2 and N 2 Reduction under the condition of mixed gas, the reduction temperature is 250 ℃, the reduction time is 2h, the obtained catalyst is marked as Ru-CNTs-5-red. The mass fraction of Ru is 2wt%, and that of carbon nanotubes is 98wt%.

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Abstract

The invention relates to preparation of a catalyst with metal nanoparticles loaded on the inner wall of a silicon dioxide nanotube and application of the catalyst in amide hydrogenation reduction. The catalyst provided by the invention takes a silicon dioxide nanotube as a carrier, the active component is one or two of Ru, Rh, Pd and Pt metal elements, and prepared metal nanoparticles are loaded in the silicon dioxide nanotube. The supported catalyst prepared by the invention shows good catalytic activity on preparation of organic amine through amide hydrogenation reduction.

Description

technical field [0001] The invention relates to the application of a catalyst in which metal nanoparticles are supported on the inner wall of silicon dioxide nanotubes in the hydrogenation reduction of amides. Background technique [0002] Organic amines play an important role in the preparation of medicines, dyes, pesticides, and some advanced materials. At the Roundtable Pharmaceutical Conference first established in 2005, the environmentally friendly preparation of organic amines from amides was listed as one of the three most desirable reactions. At present, the preparation of organic amines mainly includes the reductive amination of aldehydes, ketones, and alcohols, the reduction of nitriles and nitro compounds, and the hydrogenation reduction of amides. Since the preparation of organic amines from amides has the advantages of simple reaction pathways and the ability to prepare primary, secondary, and various organic amines, more and more researchers have paid attentio...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J23/44B01J23/42C07C211/17C07C209/50
CPCB01J23/462B01J23/44B01J23/42C07C209/50C07C211/17Y02P20/584
Inventor 王爱琴张悦刘菲张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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