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Preparing method and catalytic application of ruthenium nanocomposite

A technology of catalysts and nanoparticles, applied in catalytic reactions, organic compound/hydride/coordination complex catalysts, preparation of sulfonamides, etc.

Active Publication Date: 2016-07-20
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Preparation of homogeneously dispersed ultra-small metal nanoparticle catalysts using cucurbit rings and reduced graphene oxide as co-supports and protective agents has not been reported yet

Method used

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  • Preparing method and catalytic application of ruthenium nanocomposite
  • Preparing method and catalytic application of ruthenium nanocomposite
  • Preparing method and catalytic application of ruthenium nanocomposite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] For the preparation of Ru / CB / rGO, 0.2 mL (0.1 mmol / mL) RuCl 3 Add the aqueous solution of 300mL deionized water, and adjust its pH value to 7 with 0.1M aqueous sodium hydroxide solution; Body salt solution, stirred for 4 hours to a uniform suspension; 190mgNaBH 4 Dissolve in 200mL ethanol and quickly add it dropwise to the above suspension; keep stirring in a closed environment for 3 hours, then centrifuge, wash twice with water and once with ethanol. After drying, it was dispersed in ethanol, and the product was observed by transmission electron microscopy as ultra-small Ru nanoparticles (Ru / CB / rGO) with a diameter of 1.25±0.25nm and uniform dispersion. The result of plasma emission spectrometry (ICP) analysis showed that the Ru content was 2%.

Embodiment 2

[0028] 3mL (0.1mmol / mL) RuCl 3 Add the aqueous solution of 300mL deionized water, and adjust its pH value to 7 with 0.1M aqueous sodium hydroxide solution; Body salt solution, after stirring for 4 hours to a uniform suspension; 2.85gNaBH 4 Dissolve in 400mL ethanol and quickly add it dropwise to the above suspension; keep stirring in a closed environment for 3 hours, then centrifuge, wash twice with water and once with ethanol. The results of ICP analysis showed that the Ru content was 30%.

Embodiment 3

[0030] All steps were the same as in Example 1, except that the six-membered melon ring was replaced by an eight-membered melon ring to obtain Ru / CB[8] / rGO, and the ICP analysis results showed that the Ru content was 12%.

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Abstract

The invention provides a method of preparing a ruthenium nano-particle catalyst with cucurbit urils and reduction-oxidation graphene serving as common carriers in a synthesis mode, and the catalyst is used for catalytic synthesis of an aromatic sulfamide compound. The chemical component of the nano-particle catalyst is ruthenium, cucurbit urils and reduction-oxidation graphene, cucurbit urils and reduction-oxidation graphene serve as the common carriers, reduction-oxidation graphene is effectively prevented from agglomerating by means of the electrostatic interaction and volume effect of cucurbit urils, and the prepared ultra-small Ru nano-particles are uniform in particle size and are dispersed evenly. The prepared nano-particle catalyst is high in catalytic activity and stability and capable of efficiently catalyzing a sulfamide and aromatic alcohol reaction to prepare the aromatic sulfamide compound. The catalyst can be repeatedly used while activity is not reduced obviously. The method has the advantages of being simple in synthesis, convenient to operate, wide in application range, mild in preparation condition, simple and low in cost, and special equipment is not needed.

Description

technical field [0001] The invention relates to a method for synthesizing ultra-small ruthenium nanoparticles with uniform dispersion and uniform particle size by using melon rings and reduced graphene oxide as co-carriers. The reduced graphene oxide is intercalated by using the electrostatic interaction and the volume effect of the melon ring to obtain the reduced graphene oxide without agglomeration. Cucurbit rings and reduced graphene oxide are used as co-supports and protective agents to effectively limit the agglomeration and growth of ruthenium nanoparticles, resulting in ruthenium nanocatalysts with excellent performance in organic catalysis. The invention belongs to the field of catalytic materials. Background technique [0002] Efficient construction of new carbon-nitrogen bonds has always been a hot spot in the field of organocatalysis. Aromatic sulfonamide compounds containing carbon-nitrogen bonds are the basic building blocks of many drugs and organic light-em...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C303/40C07C311/16
CPCC07C303/40B01J31/063B01J2231/4283B01J35/393B01J35/399C07C311/16
Inventor 吴冬霜曹荣曹敏纳
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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