Preparation method of bifunctional Pickering emulsion catalyst

A functional and catalyst technology, applied in the field of preparation of dual-functional Pickering emulsion catalysts, can solve the problems of long reaction time, large amount of catalyst and high reaction temperature, and achieves the effects of simple operation, low preparation cost and optimized reaction conditions.

Pending Publication Date: 2020-05-26
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved in the research of the present invention is aimed at the shortcomings of high reaction temperature, long reaction time and large catalyst consumption in the Pickering emulsion catalyst prepared by graphene oxide (GO) immobilized organic amine in the catalyzed Knoevenagel condensation reaction. , invented a green, simple and easy-to-prepare bifunctional Pickering emulsion catalyst preparation method, which can efficiently catalyze the Knoevenagel condensation reaction at room temperature

Method used

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  • Preparation method of bifunctional Pickering emulsion catalyst
  • Preparation method of bifunctional Pickering emulsion catalyst
  • Preparation method of bifunctional Pickering emulsion catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0030] A preparation method of a dual-functional Pickering emulsion catalyst, using a dual-functionalized graphene oxide material, benzaldehyde and solvent water to form a Pickering emulsion with more superior properties, and using the dual-functional emulsion catalyst to catalyze benzaldehyde at room temperature Knoevenagel condensation reaction with malononitrile.

[0031] The method is carried out according to the following steps:

[0032](1) Weigh 0.2g of graphite oxide into a round-bottomed flask containing 100mL of tetrahydrofuran (THF) solution, then dropwise add 1.8g of 3-aminopropyltrimethoxysilane (APTMS) and 0.2g of 3-methyltrimethoxysilane Oxysilane (MTMS), followed by ultrasound three times (180W, 60Hz), each time for 30min, with an interval of 5min. Put the solution in the bottle under N 2 Under the protection of the atmosphere, reflux and stir at 70°C for 24h, then filter and wash with absolute ethanol several times, and finally vacuum-dry at 50°C for 6h to ob...

Embodiment 2

[0036] Weigh 0.2g of graphite oxide and add it to a round-bottomed flask containing 100mL of THF solution, then dropwise add 1.8g of 3-aminopropyltrimethoxysilane and 0.2g of 3-methyltrimethoxysilane, then sonicate three times (180W , 60Hz), 30 minutes each time, with an interval of 5 minutes in between. Next, put the bottle solution in N 2 Under the protection of atmosphere, reflux and stir at 70°C for 24h, then filter and wash with absolute ethanol for several times, and finally vacuum-dry at 50°C for 6h to obtain bifunctional graphene oxide. Then weigh 20mg of bifunctional graphene oxide and add it to a 50mL round bottom flask, then add 3mL of water and 1.5mL of benzaldehyde, then sonicate for 5min (180W, 60Hz), and mechanically stir at 800rpm for 5min after sonication to prepare Bifunctional Pickering emulsion catalyst, denoted as Emulsion 1.

Embodiment 3

[0038] Weigh 0.2g of graphite oxide and add it to a round-bottomed flask containing 100mL of THF solution, then dropwise add 1.8g of 3-aminopropyltrimethoxysilane and 0.2g of 3-methyltrimethoxysilane, then sonicate three times (180W , 60Hz), 30 minutes each time, with an interval of 5 minutes in between. Next, put the bottle solution in N 2 Under the protection of atmosphere, reflux and stir at 70°C for 24h, then filter and wash with absolute ethanol for several times, and finally vacuum-dry at 50°C for 6h to obtain bifunctional graphene oxide. Then weigh 20mg of bifunctional graphene oxide and add it to a 50mL round bottom flask, then add 4mL of water and 1.5mL of benzaldehyde, then sonicate for 5min (180W, 60Hz), and mechanically stir at 800rpm for 5min after sonication to prepare Bifunctional Pickering emulsion catalyst, denoted as Emulsion 2.

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Abstract

The invention belongs to the field of chemical engineering, and relates to a preparation method of a bifunctional Pickering emulsion catalyst, which comprises the following steps of: carrying out ultrasonic treatment and mechanical stirring on a bifunctional graphene oxide material, benzaldehyde and water to prepare the bifunctional Pickering emulsion catalyst. The bifunctional graphene oxide (GO-NH2-Si) is prepared by simultaneously modifying graphene oxide (GO) by utilizing 3-aminopropyltrimethoxysilane (APTMS) and 3-methyltrimethoxysilane (MTMS). The preparation method of the Pickering emulsion catalyst is simple, the preparation cost is low, the catalytic activity is high, and compared with an emulsion catalyst prepared by only utilizing APTMS modified GO (GO-NH2) in the prior art, theconversion rate of benzaldehyde is increased by about 24% in a Knoevenagel reaction.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a Knoevenagel condensation reaction catalyst and its preparation technology, in particular to a preparation method of a Pickering emulsion catalyst with dual functions. Background technique [0002] The Knoevenagel condensation reaction is one of the most valuable reactions for forming carbon-carbon double bonds in industry, and its products α, β-unsaturated carbonyl compounds have a wide range of applications in industry, agriculture and biomedicine. Traditional homogeneous catalysts such as organic amines, piperidines, etc. can catalyze the reaction to obtain higher product yields, but their inherent homogeneous nature makes it difficult to separate the catalyst from the product. Therefore, in the Knoevenagel reaction, heterogeneous catalysts are usually used . Most of the Knoevenagel condensation reactions are carried out in organic solvents, and the use of organic solvents may...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C253/30C07C255/33
CPCB01J31/069C07C253/30B01J2231/341C07C255/33
Inventor 李永昕张博王飞李东升薛冰
Owner CHANGZHOU UNIV
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