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Preparation method and application of palladium cluster catalyst

A catalyst and cluster technology, which is applied in the preparation of noble metal cluster catalysts and its catalytic synthesis of fine organic chemicals, to achieve high product selectivity, improve stability, and overcome agglomeration

Pending Publication Date: 2022-03-11
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Another object of the present invention is to provide a more environmentally friendly, efficient and economical method for the selective catalytic hydrogenation of enols in view of the shortcomings of the existing methods for the selective catalytic hydrogenation of acetylenic alcohols as raw materials for the synthesis of enols (as shown below)

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  • Preparation method and application of palladium cluster catalyst
  • Preparation method and application of palladium cluster catalyst
  • Preparation method and application of palladium cluster catalyst

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Effect test

Embodiment 1

[0029] A kind of preparation method of Pd cluster catalyst, concrete method is as follows: 500mg trimesaldehyde, 500mg (1R, 2R)-cyclohexanediamine, 10 μ L CF 3 Add 10mL CH to COOH 2 Cl 2 , stir to dissolve evenly, and let the mixed solution stand at room temperature for 1-7 days, then centrifuge the crystallized solid powder and dissolve it in 50mL CHCl 2 / CH 3 OH mixture (1:1, v / v); after the solution is clarified, add 0.5 g of sodium borohydride and stir continuously at room temperature for 12 hours, and adopt centrifugal separation and vacuum drying at room temperature to obtain a white powdery organic molecular cage RCC3; dissolve 100mg RCC3 in 6mL acetone, let it stand at room temperature for 12 hours, collect crystals, wash with acetone (2×100mL) to obtain organic molecular cage AT-RCC3; dissolve 60mg paraformaldehyde in 10mL CH 3 OH, stirred at 70°C, when the solution was clear, the CH of RCC33 OH solution was added to the above solution, and a white precipitate was ...

Embodiment 2

[0031] A kind of preparation method of Pd cluster catalyst, specific method is as follows: RCC3 molecular cage 100mg among the embodiment 1 is stirred and dispersed in 200mL deionized water, after continuous stirring, dropwise add 22mmol Pd(OAc) 2 10mL of dichloromethane solution, stirring continuously for 12h; in ice-water bath, add 4mg of newly prepared NaBH dropwise 4 40 mL of the aqueous solution was stirred vigorously for 12 h, collected by centrifugation, washed 5 times with water, and dried in vacuum at room temperature for 3 h to obtain the Pd cluster-supported catalyst Pd@RCC3.

Embodiment 3

[0033] A kind of preparation method of Pd cluster catalyst, specific method is as follows: the AT-RCC3 molecular cage 120mg among the embodiment 1 is stirred and dispersed in 200mL deionized water, after continuous stirring, dropwise add 22mmol Pd(OAc) 2 10mL of dichloromethane solution, stirring continuously for 12h; in ice-water bath, add 4mg of newly prepared NaBH dropwise 4 40 mL of the aqueous solution was stirred vigorously for 12 h, collected by centrifugation, washed 5 times with water, and dried in vacuum at room temperature for 3 h to obtain the Pd cluster-supported catalyst Pd@AT-RCC3.

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Abstract

The invention discloses a preparation method of a Pd cluster catalyst, and provides a method capable of loading Pd clusters in an organic molecular cage cavity in a limited range, aiming at the defect that the reaction activity of the Pd cluster catalyst is reduced due to the fact that the Pd clusters in the existing Pd cluster loaded catalyst are extremely easy to agglomerate into Pd nano-particles with relatively large particle sizes. The preparation method comprises the following steps: firstly synthesizing organic molecular cages RCC3, AT-RCC3 and FT-RCC3, and then carrying out confinement loading on Pd clusters in the cavities of the molecular cages by virtue of methods of adsorbing palladium ions and reducing NaBH4, so as to prepare Pd (at) RCC3, Pd (at) AT-RCC3 and Pd (at) FT-RCC3 catalysts; the particle size of the Pd cluster is regulated and controlled through the cavity size of the organic molecular cage, and the catalytic activity is indirectly regulated and controlled. When the Pd cluster catalyst prepared by the invention is used for catalyzing selective hydrogenation of alkynol to synthesize enol, the alkynol conversion rate is higher than 95%, and the enol selectivity is higher than 96%. According to the method, the prepared Pd cluster catalyst is high in stability, the operation is easy to control, the enol yield is high, and industrial production is easy when the Pd cluster catalyst is used for synthesizing the enol through selective catalytic hydrogenation.

Description

technical field [0001] The invention belongs to the technical field of the preparation of noble metal cluster catalysts and the application of catalytic synthesis of fine organic chemicals, and specifically relates to the preparation of Pd cluster catalysts and a method for catalyzing the high-selective hydrogenation of acetylenic alcohols to synthesize enols. Background technique [0002] Pd clusters are composed of several to dozens of Pd atoms; compared with Pd nanoparticles, Pd clusters have a smaller particle size and a higher proportion of metal atoms on the cluster surface. Therefore, in catalytic organic conversion reactions, Pd The utilization rate of atoms is higher, and the Pd cluster-supported catalyst has higher catalytic activity. However, due to the high surface energy of Pd clusters, ultrafine Pd clusters are easily aggregated into larger Pd nanoparticles, resulting in reduced catalytic activity. The existing methods to prevent the agglomeration of Pd cluste...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C29/17C07C33/03
CPCB01J31/0254B01J31/0244B01J31/0235C07C29/17B01J2231/645C07C33/03
Inventor 董正平寇金芳李剑凤赵华成高武杨黄若茵刘闯马科星
Owner LANZHOU UNIVERSITY
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