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Preparation method and application of palladium metal cluster catalyst

A metal cluster and catalyst technology, which is applied in the field of preparation of palladium metal cluster catalyst, can solve the problems of insufficient catalyst stability, need to improve selectivity, complicated catalyst preparation, etc., and achieves avoiding overhydrogenation phenomenon, excellent activity and selectivity. , the appearance of the same effect

Active Publication Date: 2022-08-05
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing commercial phenylacetylene hydrogenation catalyst is mainly palladium carbon (Pd / C) catalyst, which mainly uses the noble metal Pd, but it is expensive, and it is easy to introduce new impurity ethylbenzene through overhydrogenation of phenylacetylene. The activity and selection of the catalyst Sex needs further improvement
In 2015, Xue Duan et al. supported a series of Ni phosphides on Al2O3 substrates and found that Ni2P / Al2O3 material has good hydrogenation performance of phenylacetylene, but the selectivity of hydrogenation reaction (88.2%) still needs to be improved
However, the preparation process is complicated, the conditions are high, and the stability of the catalyst is also insufficient.
[0004] To sum up, there are still many problems in the existing catalytic system, such as complex catalyst preparation, poor stability, insufficient selectivity, etc.

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0026] 3g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 50 mL of methanol, then added to 100 mL of pre-prepared methanol solution containing 6.5 g of 2-methylimidazole, and stirred vigorously for 12 h at room temperature; the obtained precipitate was centrifuged, washed with methanol three times, and vacuum-dried at 65 °C overnight to obtain Zeolitic imidazole framework material ZIF8; then put the obtained ZIF8 in a ceramic boat, annealed at 1050 °C for 2 h in an Ar atmosphere; after the temperature dropped to room temperature, the obtained nitrogen-doped porous carbon was stored for later use.

[0027] 1.42g PdCl 2 Dissolve in aqueous hydrochloric acid containing 16 mmol of HCl and dilute the solution to 10 mL. 0.6 mL of the above solution was added to 10 mL of tetrahydrofuran, followed by 0.313 g of triphenylphosphine; after vigorous stirring for 10 min, 5 mL of an ethanol solution containing 0.08 g of sodium borohydride was added to the mixture, followed by vigorous stirring for ...

Embodiment 2

[0030] 3g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 50 mL of methanol, then added to 100 mL of pre-prepared methanol solution containing 6.5 g of 2-methylimidazole, and vigorously stirred at room temperature for 24 h; the obtained precipitate was centrifuged, washed with methanol three times, and vacuum-dried at 60 °C overnight to obtain Zeolitic imidazole framework material ZIF8; then put the obtained ZIF8 in a ceramic boat, annealed at 1000 °C for 3 h in an Ar atmosphere; after the temperature dropped to room temperature, the obtained nitrogen-doped porous carbon was stored for later use.

[0031] 1.42g PdCl 2 Dissolve in aqueous hydrochloric acid containing 16 mmol of HCl and dilute the solution to 10 mL. 0.6 mL of the above solution was added to 10 mL of tetrahydrofuran, followed by 0.313 g of triphenylphosphine; after vigorous stirring for 8 min, 5 mL of an ethanol solution containing 0.08 g of sodium borohydride was added to the mixture, followed by vigorous stirring for 6...

Embodiment 3

[0034] 3g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 50 mL of methanol, then added to 100 mL of pre-prepared methanol solution containing 6.5 g of 2-methylimidazole, and stirred vigorously for 36 h at room temperature; the obtained precipitate was centrifuged, washed with methanol three times, and vacuum-dried at 65 °C overnight to obtain Zeolitic imidazole framework material ZIF8; then put the obtained ZIF8 into a ceramic boat, and anneal at 950 °C for 4 h in an Ar atmosphere. After the temperature dropped to room temperature, the obtained nitrogen-doped porous carbon was stored for later use.

[0035] 1.42g PdCl 2 Dissolve in aqueous hydrochloric acid containing 16 mmol of HCl and dilute the solution to 10 mL. 0.6 mL of the above solution was added to 10 mL of tetrahydrofuran, followed by 0.313 g of triphenylphosphine; after vigorous stirring for 6 min, 5 mL of an ethanol solution containing 0.08 g of sodium borohydride was added to the mixture, followed by vigorous stirring f...

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Abstract

The invention relates to the field of metal cluster catalysts, and discloses a preparation method and application of a palladium metal cluster catalyst, the method comprises the following steps: S1, preparing a zeolite imidazole framework material ZIF8 through zinc nitrate and 2-methylimidazole, and annealing and heating the ZIF8 in Ar atmosphere to obtain a nitrogen-doped porous carbon material; s2, preparing a [Pd3Cl (PPh2) 2 (PPh3) 3] < + > [SbF6] <-> crystal as a reaction precursor by adopting a ligand-regulated liquid phase reduction method; and S3, dispersing the nitrogen-doped porous carbon in dichloromethane, dissolving the reaction precursor in dichloromethane, dropwise adding into the mixture, stirring, centrifuging, drying and separating out a supported sample, and annealing and heating in an Ar atmosphere to obtain the supported palladium metal cluster catalyst. According to the invention, the palladium metal cluster nano-catalyst with uniform dispersion and consistent morphology is prepared by a two-step annealing method, and the obtained catalyst shows excellent activity and selectivity on phenylacetylene hydrogenation reaction.

Description

technical field [0001] The invention relates to the field of metal cluster catalysts, in particular to a preparation method and application of a palladium metal cluster catalyst. Background technique [0002] Styrene is an important industrial raw material and the main monomer for synthesizing polystyrene resin and various synthetic rubbers. At present, styrene is mainly synthesized by catalytic dehydrogenation of ethylbenzene and co-oxidation of ethylbenzene. However, both of these synthetic methods produce phenylacetylene impurities, which can poison the catalyst of the polymerization reaction and affect the product quality. Therefore, how to completely remove phenylacetylene impurities in styrene raw materials is an important issue in modern chemical production. [0003] At present, phenylacetylene impurity removal from styrene raw materials is mainly achieved by catalytic selective hydrogenation of phenylacetylene. Existing commercial phenylacetylene hydrogenation cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C5/09C07C15/46
CPCB01J27/24C07C5/09C07C2527/24C07C15/46Y02E60/50Y02P20/584
Inventor 姚涛张伟汪思聪丁韬
Owner UNIV OF SCI & TECH OF CHINA
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