Graphene oxide supported ruthenium catalyst as well as preparation method and application thereof

A ruthenium catalyst and supported technology, which is applied in the direction of physical/chemical process catalysts, catalytic reactions, carbon-based compound preparation, etc., can solve the problems of harsh reaction conditions and many by-products, and achieve the effect of simple post-processing

Active Publication Date: 2021-02-12
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Existing reactions for the synthesis of substituted ketones generally need to be reacted under the conditions

Method used

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  • Graphene oxide supported ruthenium catalyst as well as preparation method and application thereof
  • Graphene oxide supported ruthenium catalyst as well as preparation method and application thereof
  • Graphene oxide supported ruthenium catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1 graphene oxide supported ruthenium catalyst

[0048] (1) Put 10mmol of benzotriazole, 15mmol of 2,5-dibromothiophene, and 7.5mmol of potassium tert-butoxide in a 100mL round bottom flask, add 30mL of toluene to it, place it in an oil bath at 125°C, and stir it magnetically React for 24 hours. After the reaction is completed, wait for it to cool to room temperature, collect the filtrate by suction filtration, and remove the solvent by rotary evaporation of the filtrate. Add 10 mmol 1-naphthylboronic acid, 3 mmol palladium chloride, 8 mmol potassium phosphate and 40 mL distilled water to the residue obtained. React at 110°C for 12 hours. After the reaction, extract with ethyl acetate three times, collect the organic phase, and remove the solvent by rotary evaporation to obtain 3.12 g of solid. In the presence of nitrogen, add 3.12 g of solids and 1.6 g of ruthenium trichloride into the Schlenk bottle, reflux reaction in ethylene glycol methyl ether at 120 ° C...

Embodiment 2

[0051] Embodiment 2 graphene oxide supported ruthenium catalyst

[0052] (1) Put 10mmol of benzotriazole, 17.5mmol of 2,5-dibromothiophene, and 8.5mmol of potassium tert-butoxide in a 100mL round-bottomed flask, add 35mL of toluene to it, place it in an oil bath at 130°C, and magnetically Stir the reaction for 30 hours. After the reaction is completed, wait for it to cool to room temperature, collect the filtrate by suction filtration, and remove the solvent by rotary evaporation of the filtrate. Add 12 mmol 1-naphthylboronic acid, 5 mmol palladium chloride, 10 mmol potassium phosphate and 45 mL distilled water to the obtained residue , reacted at 110°C for 16h, extracted 3 times with ethyl acetate after the reaction, collected the organic phase, and evaporated the organic matter to remove the solvent to obtain 3.84g of solid. In the presence of nitrogen, 3.84 g of solid and 2 g of ruthenium trichloride were added to the Schlenk bottle, and refluxed in ethylene glycol methyl e...

Embodiment 3

[0055] Embodiment 3 graphene oxide supported ruthenium catalyst

[0056] (1) Put 10mmol of benzotriazole, 20mmol of 2,5-dibromothiophene, and 10mmol of potassium tert-butoxide in a 100mL round bottom flask, add 40mL of toluene to it, place it in an oil bath at 140°C, and stir the reaction by magnetic force 36h, after the reaction was completed, wait for it to cool to room temperature, collect the filtrate by suction filtration, and remove the solvent by rotary evaporation of the filtrate, add 15mmol 1-naphthylboronic acid, 8mmol palladium chloride, 10mmol potassium phosphate and 50mL distilled water to the residue obtained, The reaction was carried out at ℃ for 18 hours. After the reaction was completed, it was extracted three times with ethyl acetate, the organic phase was collected, and the organic matter was rotary evaporated to remove the solvent to obtain 4.02 g of solid. In the presence of nitrogen, add 4.02 g of solid and 2.3 g of ruthenium trichloride into the Schlenk ...

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Abstract

The invention discloses a graphene oxide supported ruthenium catalyst as well as a preparation method and application thereof, and belongs to the crossing field of organic chemistry and material chemistry. According to the present invention, graphene oxide is adopted as a carrier to load a supported catalyst containing metal ruthenium, the catalyst is used for catalyzing the reaction between the alcohol and the alcohol to synthesize the substituted ketone compound, the test result shows that the catalyst provides the high catalytic activity for the reaction, and the catalyst can be recycled; and meanwhile, the catalyst can also be used for synthesizing bisphenol F under mild reaction conditions, and accords with the ideas of atom economy and green chemistry development.

Description

technical field [0001] The invention relates to a graphene oxide-supported ruthenium catalyst and a preparation method and application thereof, which belong to the cross field of organic chemistry and material chemistry. Background technique [0002] Graphene oxide is a kind of derivative of graphene, which has a planar two-dimensional sheet structure similar to graphene. Because it has a larger specific surface area that is conducive to the transportation of substances, and compared with graphene, its surface contains more active groups such as hydroxyl, carboxyl, and epoxy groups, and can be loaded by π-π stacking. Therefore, it has a bright application prospect in the fields of photoelectrocatalysis and drug carrier, so it has attracted extensive attention of many chemical and material, biological and medicinal chemists in recent years. [0003] Transition metal catalysts have received extensive attention since the last century. Among them, metal ruthenium is more stable...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J31/18C07C45/00C07C49/782C07C49/813C07C49/84C07C37/20C07C39/16
CPCB01J31/1825B01J31/226B01J2231/4205B01J2231/4288B01J2531/0241B01J2531/821C07C37/20C07C45/00C07C49/782C07C49/813C07C49/84C07C39/16Y02P20/584
Inventor 王大伟李家豪姚玮朱观鑫倪才华
Owner JIANGNAN UNIV
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