Supercritical carbon dioxide/polyethylene glycol stabilized palladium nano particle catalysis system

A technology of polyethylene glycol and carbon dioxide, applied in the direction of organic compound/hydride/coordination complex catalyst, oxidation to carbonyl compound, physical/chemical process catalyst, etc., can solve problems in the initial stage and achieve increased reaction Increased speed, reactivity, and avoidance of cross-contamination

Inactive Publication Date: 2009-12-09
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
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Problems solved by technology

Currently, scCO 2 - The application research of polymer two-phase system in catalytic reaction is still in the initial stage

Method used

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  • Supercritical carbon dioxide/polyethylene glycol stabilized palladium nano particle catalysis system

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: the preparation of the palladium catalyst that size is 2-5 nanometer

[0025] Acetic acid solution dissolved with 2,2′-dipyridylamine functionalized polyethylene glycol (21mg, 0.009mmol) was added to a two-necked flask, palladium acetate (4.1mg, 0.018mmol) was added, and stirred at room temperature for 4h for formulation bit. Then H was introduced at room temperature 2 , carry out reduction; after 20 minutes to obtain a brown-black solution, stop feeding hydrogen, add 8g PEG to remove acetic acid to obtain 2,2'-dipyridylamine functionalized polyethylene glycol-stabilized palladium catalyst of 2 to 5 nanometers.

Embodiment 2

[0026] Embodiment 2: The size is the preparation of the palladium catalyst of 5-10 nanometers

[0027] Acetic acid solution dissolved with 2,2′-dipyridylamine functionalized polyethylene glycol (21mg, 0.009mmol) was added to a two-necked flask, palladium acetate (4.1mg, 0.018mmol) was added, and stirred at room temperature for 4h for formulation bit. Then H was introduced at room temperature 2 , carry out reduction; 50 minutes later to obtain brown gray black solution, stop feeding hydrogen, add 8g PEG to remove acetic acid to obtain 2,2'-dipyridylamine functionalized polyethylene glycol stabilized palladium catalyst of 5 to 10 nanometers.

Embodiment 3

[0028] Example 3: In scCO 2 In the aerobic oxidation reaction of benzyl alcohol catalyzed by palladium nanoparticles in / PEG two-phase system, the example 1 adds substrate (2.4mmol) successively in the autoclave of 48ml, palladium catalyst (0.018mmol), then fills in the autoclave 19.8g of CO 2 and O 2 The mixed gas (the molar ratio of carbon dioxide and oxygen: 94:6) was heated to 80° C. with a heating mantle under electromagnetic stirring, and reacted for 6 hours. After the reaction, at a temperature of 70°C and a pressure of 17MPa, supercritical carbon dioxide was used to extract the substrate and product in situ at a certain rate, and a cold trap filled with isopropanol was used to absorb the tail gas at 0°C. According to GC analysis, the conversion rate of benzyl alcohol was 97%, and the selectivity of benzaldehyde was 95%.

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Abstract

The invention provides a supercritical carbon dioxide/polyethylene glycol stabilized palladium nano particle catalysis system, belonging to the technical field of catalyst application, mainly comprising the following steps: (1) using 2,2'-dipyridylamine modified polyethylene glycol as a carrier, after coordinating with palladium acetate, based on the reducer of hydrogen, reducing Pd(II) as Pd(0), obtaining Pd nano particle catalyst; (2) sequentially adding the substrate, palladium catalyst, polyethylene glycol to a high pressure kettle, and then sequentially quantitatively filling CO2, O2 in the high pressure kettle, preferably 10 g to 20 g of mixed gases of CO2 and O2, heating to the appointed temperature with the heating sleeve in the electromagnetic stirring. After the reaction is finished, in situ extracting the substrate and the product with the supercritical carbon dioxide at the temperature of 70 DEG C and preferable pressure of 16 MPa to 20 MPa, and absorbing the tail gas with the cold trap filled with isopropanol.

Description

technical field [0001] The invention relates to a two-phase catalytic system based on supercritical carbon dioxide / polyethylene glycol, especially the application of supercritical carbon dioxide in the aerobic oxidation reaction of alcohols and the separation of products, belonging to the technical field of catalyst application. Background technique [0002] The selective oxidation of alcohols to the corresponding aldehydes and ketones is one of the most versatile functional group transformation reactions in organic synthesis, and has very important applications in both fundamental research and industrial organic synthesis. At present, although there are many effective methods for realizing the conversion reaction, harsh reaction conditions or toxic oxidants are usually required, resulting in a large amount of environmental pollutants. In recent years, air, pure oxygen or H 2 o 2 As a clean oxidant, the research on catalytic oxidation of alcohols with transition metals, es...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28B01J31/22C07C45/29
CPCY02P20/54
Inventor 侯震山汪向锐冯博林珲鸿胡玉乔云香李欢
Owner EAST CHINA UNIV OF SCI & TECH
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