Preparation method of graphene loaded palladium nanoparticle composite material catalyst
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A technology of palladium nanoparticles and composite materials, which is applied in the field of preparation of graphene-supported palladium nanoparticle composite catalysts, can solve the problems of complex process, poor repeatability, high cost, etc., and achieve the effect of simple process flow, easy implementation and easy recycling
Active Publication Date: 2020-08-28
SINO PLATINUM METALS CO LTD
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Embodiment 1
[0019] (1) Impregnation process: pipette an appropriate volume of a certain concentration of palladium chloride solution, then take an appropriate amount of graphene oxide aqueous solution according to the mass ratio of the carrier to palladium of 400:1, put it into the solution, and immerse for 36 hours.
[0020] (2) Spray drying process: use a spray dryer to control the liquid flow rate of 4.0ml / min for the mixed solution obtained in (1), the atomization pressure is 0.4MPa, the inlet temperature is 180°C, and the hot air flow rate is 8.0L / min. min, carry out drying treatment, and receive the graphene oxide powder containing palladium.
[0021] (3) High-temperature reduction process: the palladium-containing graphene oxide powder obtained in (2) was reduced in a tube furnace in a hydrogen atmosphere at 500° C. for 1 hour, and the palladium-loaded graphene powder was obtained.
[0022] (4) Re-impregnation process: Weigh an appropriate amount of palladium acetate, dissolve it w...
Embodiment 2
[0026] Palladium nanoparticle-graphene catalyst of the present invention is made by following process:
[0027] (1) Impregnation process: pipette an appropriate volume of palladium chloride solution with a concentration of , and then take an appropriate amount of graphene oxide aqueous solution according to the mass ratio of the carrier to palladium as 1000:1, and put it into the solution, and immerse for 24 hours .
[0028] (2) Spray drying process: use a spray dryer to control the liquid flow rate of 6.0ml / min for the mixed solution obtained in (1), the atomization pressure is 0.3MPa, the inlet temperature is 180°C, and the hot air flow rate is 8.0L / min. min, carry out drying treatment, and receive the graphene oxide powder containing palladium.
[0029] (3) High-temperature reduction process: the palladium-containing graphene oxide powder obtained in (2) was reduced in a tube furnace in a hydrogen atmosphere at 500° C. for 1 hour to obtain palladium-loaded graphene powder....
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Abstract
The invention discloses a preparation method of a graphene loaded palladium nanoparticle composite material catalyst. The preparation method comprises the following steps: (1) dipping: putting graphene oxide into a palladium chloride solution for dipping; (2) performing spray drying: carrying out spray drying treatment on a solution obtained in step (1) to obtain palladium-containing graphene oxide powder; (3) performing high-temperature reduction: performing high-temperature reduction on the palladium-containing graphene oxide powder prepared in step (2) in a H2 atmosphere to obtain palladium-containing graphene powder; (4) re-dipping: weighing a proper amount of the palladium-containing graphene powder prepared in step (3), and putting the palladium-containing graphene powder into an ethanol-water solution of palladium acetate for re-dipping; (5) performing chemical reduction: adding phenylboronic acid, bromobenzene and cesium carbonate into a solution obtained in step (4) accordingto a certain molar ratio, and carrying out chemical reduction; and (6) separating and drying to obtain the graphene loaded palladium nanoparticle catalyst with the palladium loading capacity of 1.0-2.5 wt%. The method has the advantages of simple process flow and mild conditions, and the prepared catalyst has high activity and can be repeatedly used.
Description
technical field [0001] The invention belongs to the technical field of preparation of supported noble metal catalysts, and in particular relates to a method for preparing graphene-supported palladium nanoparticle composite catalysts. Background technique [0002] Palladium-catalyzed carbon-carbon coupling reactions have a wide range of applications in organic synthesis, and have been used in pesticides, pharmaceutical intermediates, organic functional materials, liquid crystal materials, and biochemistry. According to the type of C-C coupling reaction precursor, the coupling reaction can be roughly divided into two reaction types: self-coupling and cross-coupling; the main types of cross-coupling reactions include: Suzuki-Miyaura, Heck, Hiyama, Sonogashira reactions, etc. Among them, palladium-catalyzed Suzuki-Miyaura coupling reaction between aryl boronic acid and halogenated arene has attracted much attention due to its advantages of mild reaction conditions and high selec...
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