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A kind of preparation method and application of high hydrogenation selectivity ir@mil-101(fe) catalyst

A technology of aldehyde selectivity and hydrogenation reaction, which is applied in the preparation of organic compounds, catalytic reactions, organic compound/hydride/coordination complex catalysts, etc., which can solve the complex synthesis process and the long contact distance of metal active sites , catalyst hydrogenation activity reduction and other problems, to achieve the effect of simple synthesis method, excellent selectivity and activity, and improved stability

Active Publication Date: 2022-07-12
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although such a structure can enhance the stability and recyclability of metal nanoparticles, it will also lead to a longer contact distance between reactants and metal active sites, and some of the metal active sites will be covered by MOFs, resulting in the increase of the catalyst. The hydrogen activity is reduced, and the final catalyst needs to be under high temperature and high pressure reaction conditions to catalyze hydrogenation
At the same time, the synthesis process of this method is more complicated, and dangerous gases such as hydrogen are required as reducing agents for metal salts.

Method used

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  • A kind of preparation method and application of high hydrogenation selectivity ir@mil-101(fe) catalyst
  • A kind of preparation method and application of high hydrogenation selectivity ir@mil-101(fe) catalyst
  • A kind of preparation method and application of high hydrogenation selectivity ir@mil-101(fe) catalyst

Examples

Experimental program
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Effect test

Embodiment 1I

[0056] Example 1 Preparation of Ir@MIL-101(Fe) Heterogeneous Catalyst

[0057] (1) Preparation of Ir nanoclusters: Dissolve 30 mg of hydrated iridium trichloride and 50 mg of PVP in 10 ml of EG (ethylene glycol), stir at room temperature for 30 minutes (about 25°C, and stir at 500 rpm) ) and transfer the mixture to a 20 ml glass bottle. The glass bottle was sealed and reacted in a pre-heated 180°C oil bath for 3 hours. After the reaction solution was cooled to room temperature, the product was collected by centrifugation at 11,000 rpm for 5 minutes. Mixed solvent (ethanol: acetone = 1:1) The product was washed twice, and the obtained Ir nanoclusters were redispersed in 20 ml of DMF (concentration of 0.67 mg / ml) for use.

[0058] (2) Preparation of Ir@MIL-101(Fe): 200 mg of ferric chloride hexahydrate and 116 mg of terephthalic acid were dissolved in 45 mL of DMF, and then 5 mL of the Ir nanoclusters synthesized in step (1) were added The solution was stirred at room temperat...

experiment example 1I

[0079] Experimental Example 1. Activity and Selectivity Analysis of Ir@MIL-101(Fe) Heterogeneous Catalyst for Selective Catalytic Hydrogenation

[0080] The model molecule of α,β-unsaturated aldehyde, cinnamaldehyde, was selected as the catalytic substrate to compare the performance of different catalysts (the catalysts prepared in Example 1 and Comparative Examples 1-3, Ir nanoclusters, and MIL-101(Fe)). Catalytic activity and product selectivity. Its catalytic principle is as Figure 11 As shown, cinnamaldehyde is hydrogenated into cinnamyl alcohol, hydrogenated cinnamaldehyde and phenylpropanol under the action of catalyst and hydrogen, and the ideal product is cinnamyl alcohol.

[0081] Heterogeneous catalytic hydrogenation reaction conditions are as follows: the dosage of the catalyst is 15 mg, and the dosage of cinnamaldehyde is 0.1 mmol, both of which are added to the mixed solution of 2.5 ml of water and 2.5 ml of isopropanol, and ultrasonically mixed for 10 minutes t...

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Abstract

The invention belongs to the technical field of selective hydrogenation, and in particular relates to a preparation method and application of a high hydrogenation selectivity Ir@MIL-101(Fe) catalyst. The invention encapsulates Ir nanoclusters in a hollow space through a simple in-situ growth method. In the cavity of the MIL-101(Fe), and the Ir nanoclusters are mainly distributed on the near surface of the MIL-101(Fe), the synthesis method of the invention is simple, and only two steps are needed to obtain the metal nanoclusters encapsulated in the MOFs hollow. The structure of the cavity, and no special atmosphere is required in the reaction process, the obtained Ir@MIL‑101(Fe) is a hollow structure with high mesoporosity, which can be catalytically hydrogenated α, β‑ at room temperature and pressure Unsaturated aldehydes have high catalytic activity and good recycling ability, and are excellent catalysts for the selective hydrogenation of α, β-unsaturated aldehydes to prepare unsaturated alcohols, with excellent selectivity and activity.

Description

technical field [0001] The invention belongs to the technical field of selective hydrogenation, in particular to a preparation method and application of a high hydrogenation selectivity Ir@MIL-101(Fe) catalyst. Background technique [0002] In recent years, the selective hydrogenation of α,β-unsaturated aldehydes to obtain relatively single products has become a research hotspot, because both C=C double bond hydrogenation products and C=O double bond hydrogenation products can be used. It is used in the fields of reaction intermediates, perfumes, food processing and so on. Since C=O double bonds are more stable than C=C double bonds in thermodynamics, it is still difficult to obtain unsaturated alcohols by highly selective hydrogenation of C=O bonds. Ir has a broad d-band and is highly active for the hydrogenation of α,β-unsaturated aldehydes, but due to the fact that C=C bonds and C=O bonds can simultaneously be on larger unoccupied d orbitals Adsorption and activation, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28B01J31/22B01J35/10C07C29/141C07C33/32C07C33/48C07D307/42C07C33/03C07C41/26C07C43/23
CPCB01J31/28B01J31/1691C07C29/141C07D307/42C07C41/26B01J2531/842B01J2531/0213B01J2231/643B01J35/23B01J35/647C07C33/32C07C33/483C07C33/03C07C43/23Y02P20/584
Inventor 李光琴刘千刘庆林
Owner SUN YAT SEN UNIV