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A kind of spirofluorenepyridine palladium nanoparticles and preparation method thereof

A technology of spirofluorenpyridine palladium and spirofluorenpyridine, which is applied in the field of spirofluorenpyridine palladium nanoparticles and its preparation, can solve the problems of shape, distribution and particle size of nano-catalysts, and achieve low cost, stable performance and high reactivity Effect

Active Publication Date: 2016-05-18
铜陵市清华宝能源设备有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although nanocatalysts have achieved some development and application results, there are still problems in controlling the shape, distribution and particle size of nanocatalysts.

Method used

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  • A kind of spirofluorenepyridine palladium nanoparticles and preparation method thereof
  • A kind of spirofluorenepyridine palladium nanoparticles and preparation method thereof
  • A kind of spirofluorenepyridine palladium nanoparticles and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Quickly add 10mL of 5.0mmol / L palladium chloride aqueous solution to 10mL of 5.0mmol / L spirofluorenepyridine ethylene glycol solution into a 50mL three-neck flask, stir vigorously at room temperature for 15 minutes, and then carry out microwave reflux reaction for 20 Minutes, cooled and aged at room temperature for 3 hours. The aged product was centrifuged, and the precipitate was washed three times with deionized water and ethanol, ultrasonically dispersed, and dried to obtain the spirofluorenepyridine palladium nanoparticles. Observe the morphology of the nanoparticles with a scanning electron microscope, such as figure 2 As shown, the particle size of nanoparticles is 20-100nm.

[0032] Wherein, the preparation method of the spirofluorenpyridine comprises: 2,2',7,7'-tetrabromo-9,9'-spirobifluorene (3.0mmol, 1.91g), 4-pyridineboronic acid (9.0mmol, 1.12g), potassium carbonate (40.0mmol, 5.52g), toluene / ethanol / water (80mL / 30mL / 20mL) were added to a 250mL three-neck...

Embodiment 2

[0034] Quickly add 10mL of 10mmol / L palladium chloride aqueous solution into a 50mL three-necked flask containing 10mL of 5.0mmol / L spirofluorenepyridine ethyl acetate solution, stir vigorously at room temperature for 15 minutes, then carry out microwave reflux reaction for 40 minutes, cool Then aged at room temperature for 5h. The aged product was centrifuged, and the precipitate was washed three times with deionized water and ethanol, ultrasonically dispersed, and dried to obtain the spirofluorenepyridine palladium nanoparticles. The morphology of the nanoparticles was observed with a scanning electron microscope.

Embodiment 3

[0036] Quickly add 10mL of 5.0mmol / L palladium acetate aqueous solution into a 50mL three-neck flask containing 10mL of 1.0mmol / L spirofluorene pyridine glycol solution, stir vigorously at room temperature for 15 minutes, and then carry out microwave reflux reaction for 30 minutes, After cooling, it was aged at room temperature for 4 hours. The aged product was centrifuged, and the precipitate was washed three times with deionized water and ethanol, ultrasonically dispersed, and dried to obtain the spirofluorenepyridine palladium nanoparticles. The morphology of the nanoparticles was observed with a scanning electron microscope.

[0037]With embodiment 1, the spirofluorene pyridine palladium nano-particle prepared by embodiment 2 and embodiment 3 is example, carry out catalytic reaction:

[0038] Use the spirofluorenepyridine palladium nanoparticles prepared in the above example 1 as a catalyst to carry out the catalytic reaction, the reaction conditions are: 1.0mmol 4-bromox...

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Abstract

The invention discloses a spirofluorene pyridine palladium nanoparticles and a preparation method thereof. The method is as below: adding a certain amount of metal salt solution into the organic ligand containing pyridine units, stirring for 1-3 h at a certain temperature, aging for 3-5 h, conducting centrifugal separation, washing and drying to obtain corresponding metal-ligand nanoparticles. The preparation process is simple, low in cost and suitable for mass production; and by using different solvents, controlling the amount of reactants, reaction time and temperature, the method achieves effective regulation on particle size and dispersion of spirofluorene pyridine palladium nanoparticles. The prepared spirofluorene pyridine palladium nanoparticles are functionalized nanoparticles containing palladium, have stable performance, can be used for the catalysis of C-C bond coupling reaction, and have high catalytic efficiency and yield reaching 90-99%. Therefore, the spirofluorene pyridine palladium nanoparticles have broad application prospects in the field of catalysis.

Description

technical field [0001] The invention belongs to the field of metal nanoparticle catalysis, and in particular relates to a spirofluorenepyridine palladium nanoparticle used for catalytic reaction and a preparation method thereof. Background technique [0002] Broadly speaking, nanomaterials refer to materials with crystal, amorphous, quasi-crystal and interface layer structures in which any one-dimensional scale is less than 100 nm. When the small particle size is added to the nanometer level, it has volume effect, surface effect, quantum size effect and macroscopic quantum tunneling effect. So that it has singular mechanical, electrical, optical, thermal, chemical activity, catalytic and superconducting properties, making nanomaterials have important application value in various fields. As the size of nanoparticles decreases, the specific surface area increases, the number of surface atoms increases, and the coordination unsaturation of surface atoms leads to a large number...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/26B82Y40/00B01J31/22C07B37/00C07C253/30C07C255/50C07C15/52C07C15/14C07C1/32C07C2/86
CPCB01J31/182B01J31/22B01J2231/4211B01J2231/4261B01J2531/824B82Y40/00C07B37/00C07C1/321C07C2/86C07C253/30C07C2531/22C07D213/26C07C255/50C07C15/52C07C15/14
Inventor 赵秀华李星赵亚云刘素娟康晶燕
Owner 铜陵市清华宝能源设备有限责任公司
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