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A kind of fluorenone pyridine nickel nanocluster and preparation method thereof

A technology of fluorenone pyridine and nanoclusters, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of complex synthesis process, environmental pollution, high price, etc., and achieve efficient catalytic coupling reaction and electron delocalization The effect of strong resistance and good catalytic performance

Active Publication Date: 2018-09-28
滨州市科创孵化器有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional catalysts are mainly Pd(PPh 3 ) 4 Such catalysts have high catalytic activity and a wide range of substrate choices, but they are prone to aryl exchange reactions of aromatic hydrocarbons, palladium black is easily formed during the reaction process, the synthesis process is complex, difficult, expensive, and phosphine complexes The body is sensitive to air and moisture, and needs to be in an inert gas atmosphere to effectively catalyze the reaction and pollute the environment. Therefore, in order to find new efficient and cheap catalysts, researchers have been making unremitting efforts.

Method used

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  • A kind of fluorenone pyridine nickel nanocluster and preparation method thereof
  • A kind of fluorenone pyridine nickel nanocluster and preparation method thereof
  • A kind of fluorenone pyridine nickel nanocluster and preparation method thereof

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Effect test

Embodiment 1

[0023] Under vigorous stirring, the isopropanol solution of fluorenone pyridine (10mmol / L, 15mL) was slowly added dropwise to nickel nitrate aqueous solution (5mmol / L, 15mL), continued vigorous stirring and reacted at 60°C for 60min, after the reaction The mixed system was ultrasonically dispersed for 30 minutes, centrifuged, and the supernatant was discarded to obtain a precipitate; the obtained precipitate was washed with deionized water and ethanol, ultrasonically dispersed, centrifuged, and the supernatant was discarded to remove free ions and unsaturated coordinated organic ligands, and then vacuum-dry the lower precipitate to obtain the fluorenone pyridine nickel nanocluster. The morphology of the nanoclusters was observed with a scanning electron microscope, as shown in figure 1 shown.

Embodiment 2

[0025] Under vigorous stirring, the propanol solution of fluorenone pyridine (20mmol / L, 15mL) was slowly added dropwise to nickel chloride aqueous solution (5mmol / L, 15mL), continued vigorous stirring and reacted at 90°C for 30min, after the reaction The mixed system was ultrasonically dispersed for 30 minutes, centrifuged, and the supernatant was discarded to obtain a precipitate; the obtained precipitate was washed with deionized water and ethanol, ultrasonically dispersed, centrifuged, and the supernatant was discarded to remove free ions and unsaturated coordinated organic ligands, and then vacuum-dry the lower precipitate to obtain the fluorenone pyridine nickel nanocluster. The morphology of the nanoclusters was observed with a scanning electron microscope.

Embodiment 3

[0027] Under vigorous stirring, the ethanol solution of fluorenone pyridine (20mmol / L, 15mL) was slowly added dropwise to nickel acetate aqueous solution (10mmol / L, 15mL), continued vigorous stirring and reacted at 90°C for 60min, and mixed The system was ultrasonically dispersed for 30 minutes, centrifuged, and the upper layer was discarded to obtain a precipitate; the obtained precipitate was washed with deionized water and ethanol, ultrasonically dispersed, and centrifuged, and the upper layer was discarded to remove free ions and uncoordinated organic ligands, and then vacuum-dry the lower precipitate to obtain the fluorenone pyridine nickel nanoclusters. The morphology of the nanoclusters was observed with a scanning electron microscope.

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Abstract

The invention discloses a fluorenone nickel pyridine nano-cluster and a method for preparing the same. The fluorenone nickel pyridine nano-cluster and the method have the advantages that fluorenone pyridine organic ligand solution is added into metal salt solution drop by drop, reaction products are ultrasonically dispersed after reaction is completely carried out, are centrifugally separated from one another, are washed and are dried under vacuum conditions to obtain the ligand-metal nano-cluster, procedures for preparing the fluorenone nickel pyridine nano-cluster are simple, and the fluorenone nickel pyridine nano-cluster is low in cost; solvents, the concentration of reactants, the reaction time and the temperatures can be changed, and accordingly the morphology of the fluorenone nickel pyridine nano-cluster can be effectively regulated and controlled; C-C cross coupling reaction can be efficiently catalyzed by the fluorenone nickel pyridine nano-cluster prepared by the aid of the method, the yield can reach 70% at least, and accordingly the fluorenone nickel pyridine nano-cluster can be widely applied to the field of catalysis.

Description

technical field [0001] The invention belongs to the field of metal-organic nanocomposite materials, and in particular relates to a fluorenone pyridine nickel nanocluster for catalyzing a carbon-carbon cross-coupling reaction and a preparation method thereof. Background technique [0002] Carbon-carbon cross-coupling reaction is one of the most important methods in organic synthesis and one of the most effective methods for the synthesis of biaryl compounds. It has always been a research hotspot in the fields of catalytic chemistry, organic chemistry and material chemistry. Traditional catalysts are mainly Pd(PPh 3 ) 4 Such catalysts have high catalytic activity and a wide range of substrate choices, but they are prone to aryl exchange reactions of aromatic hydrocarbons, palladium black is easily formed during the reaction process, the synthesis process is complex, difficult, expensive, and phosphine complexes The body is sensitive to air and moisture, and needs to be in an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/04B01J31/22C07C43/205C07C43/215C07C41/30C07C15/54C07C2/88B82Y40/00B82Y30/00
CPCB01J31/22B01J2231/4211B01J2231/4261B01J2231/4266B01J2531/847B82Y30/00B82Y40/00C07C2/88C07C41/30C07F15/045C07C43/205C07C43/215C07C15/54
Inventor 赵亚云李星
Owner 滨州市科创孵化器有限公司
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