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Spirofluorene copper pyridine micro-nano particle and preparation method thereof

A technology of micro-nano particles and copper spirofluorene pyridine, which is applied in the field of metal micro-nano particle catalysis, can solve the problems of no proposed catalytic coupling reaction efficiency, no in-depth research, etc., and achieves high reaction activity, strong delocalization, and broad application. Foreground effect

Inactive Publication Date: 2013-11-20
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no in-depth study on whether the structure, size and morphology of copper nanomaterials will affect the catalytic performance, let alone how to design copper nanocatalysts to improve the efficiency of catalytic coupling reactions
[0005] Secondly, there is still a certain gap between the catalytic activity of copper micro-nano materials and palladium catalysts.

Method used

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  • Spirofluorene copper pyridine micro-nano particle and preparation method thereof
  • Spirofluorene copper pyridine micro-nano particle and preparation method thereof
  • Spirofluorene copper pyridine micro-nano particle and preparation method thereof

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Effect test

Embodiment 1

[0030] Take 10mL of 10mmol / L copper nitrate aqueous solution and 10mL of 10mmol / L spirofluorenepyridine (tpsf for short) ethanol solution respectively, put them into a 50mL 19-necked Erlenmeyer flask, stir vigorously at 20°C for 10h, and age the blue suspension at room temperature 3h. The product obtained by the reaction was centrifuged, the clear liquid was discarded, and the remaining precipitate was washed three times with deionized water and ethanol respectively, ultrasonically dispersed, and dried to obtain spirofluorenpyridine copper micro-nano particles. The product was observed with a scanning electron microscope (SEM), see figure 1 , the product is flaky micro-nano crystals with a size of about 200-800nm.

[0031] Wherein, the preparation method of the spirofluorenpyridine comprises: 2,2′,7,7′-tetrabromo-9,9′-spirobifluorene (3mmol, 1.91g), 4-pyridineboronic acid (9mmol, 1.12g ), potassium carbonate (20mmol, 2.76g), and toluene / ethanol / water (80mL / 40mL / 20mL) were ad...

Embodiment 2

[0033] Take 10mL of 100mmol / L copper chloride aqueous solution and 10mL of 25mmol / L tpsf dichloromethane solution respectively, place them in a 50mL 19-necked Erlenmeyer flask, stir vigorously at 80°C for 30min, and age the blue suspension at room temperature for 10h. The product obtained by the reaction was centrifuged, the clear liquid was discarded, and the remaining precipitate was washed three times with deionized water and ethanol respectively, ultrasonically dispersed, and dried to obtain spirofluorenpyridine copper micro-nano particles. The product was observed with a scanning electron microscope (SEM), see figure 1 , the product is a flaky nanocrystal with a size of about 200-800nm.

Embodiment 3

[0035] Take 10mL of 30mmol / L copper sulfate aqueous solution and 10mL of 20mmol / L tpsf ethanol solution respectively, place them in a 50mL 19-necked Erlenmeyer flask, stir vigorously at 50°C for 4h, and age the blue suspension at room temperature for 6h. Centrifuge the obtained product, discard the clear liquid, wash the remaining precipitate with deionized water and ethanol three times, ultrasonically disperse, and dry to obtain spirofluorenpyridine copper micro-nano particles with a size of about 200-800nm .

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Abstract

The invention discloses a spirofluorene copper pyridine micro-nano particle and a preparation method thereof. The preparation method of the spirofluorene copper pyridine micro-nano particle comprises the following steps of: adding a certain amount of metal salt solution into organic ligand containing end-ground nitrogen atoms; stirring for 0.5-10 hours at a certain temperature; ageing for 1-10 hours, centrifugally separating, washing and drying to obtain the corresponding metal-ligand micro-nano particle. Moreover, the application of the micro-nano particle in C-C (Carbon-Carbon) coupling reaction is successfully researched. The preparation method disclosed by the invention can be used for preparing different metal-ligand micro-nano particles, and can be used for effectively adjusting the size of the particle diameter and the surface smoothness to obtain sheet metal-ligand micro-nano particles which are uniform in particle diameter, different in surface smoothness and excellent in physical and chemical performances. According to the catalysis experiment, the metal-ligand micro-nano particle which is prepared by the method disclosed by the invention has good catalytic activity when being used as a catalyst, and has a wide application prospect in the catalytic field. In the whole preparation process, the operation is simple, the material cost is low and the device investment is less, therefore, the spirofluorene copper pyridine micro-nano particle is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of metal micro-nano particle catalysis, and in particular relates to a spirofluorenepyridine copper micro-nano particle for catalyzing C-C coupling reaction and a preparation method thereof. Background technique [0002] Nanocatalysis is a fascinating and promising field in nanoscience and nanochemistry. In recent years, a large number of studies on nanoparticle catalysts have shown that nanoparticles, as catalysts, exhibit very high catalytic activity and selectivity. This is because the nanoparticle size is small, the percentage of surface atoms is large, the bonding state and electronic state of the surface are different from those inside the particle, and the incomplete coordination of the surface atoms leads to an increase in the active sites on the surface, which makes it suitable as a catalyst. Basic conditions. At the same time, as far as the surface morphology of nanoparticles is concerned, as the particle ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/127B01J31/22C07C43/205C07C43/225C07C41/30C07C22/08C07C17/263
Inventor 张洁李星赵亚云赵秀华康晶燕
Owner NINGBO UNIV
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