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Meso-porous iridium pyridine heterogeneous catalyst, and preparation method and application thereof

A heterogeneous catalyst, catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of low chemical and thermal stability, waste of resources environment , difficult to recycle and other problems, to achieve high chemical and thermal stability, wide application, eliminate the effect of reaction substrate diffusion

Inactive Publication Date: 2016-01-20
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing homogeneous catalysts have disadvantages such as low chemical and thermal stability, high cost, and difficulty in recycling, resulting in waste of resources and environmental pollution.

Method used

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  • Meso-porous iridium pyridine heterogeneous catalyst, and preparation method and application thereof
  • Meso-porous iridium pyridine heterogeneous catalyst, and preparation method and application thereof
  • Meso-porous iridium pyridine heterogeneous catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Example 1: Preparation of mercapto-functionalized mesoporous silica foam matrix (SH-MCF):

[0060] Mix P123 (4.000g) and hydrochloric acid solution (150mL1.6mol / L), then stir at 37°C for 2h until the solution becomes clear, then add 1,3,5-trimethylbenzene (4.6 mL), ammonium fluoride (0.0460g), then stirred at a temperature of 37°C for 1h; then added TEOS (7.34mL) dropwise to the solution, and then stirred at a temperature of 40°C for 4h; MPTMS (1.15mL) was added dropwise to the mixture, and aged for 20h under medium-speed stirring; then the mixture was poured into a polytetrafluoroethylene-lined autoclave, and then aged at a temperature of 100°C 24h; then the mixture was separated by filtration, washed with ethanol, and then dried in vacuum at 80°C for 12h to obtain a white powder; finally, the white powder was dispersed in a mixture of hydrochloric acid and ethanol (200mL, volume ratio 2:100) solution, and then refluxed at a temperature of 80° C. for 4 h; centrifuged ...

Embodiment 2

[0061] Embodiment 2: the preparation of homogeneous iridium pyridine catalyst (IrL):

[0062] Diisopropylammonia (0.8mL), n-butyllithium n-hexane (3.5mL, 1.6mol / L) and anhydrous tetrahydrofuran (10mL) were mixed, then stirred at -78°C under nitrogen protection for h; Add 4,4'-dimethyl-2,2'-bipyridine (1g) and anhydrous tetrahydrofuran (45mL) to the mixed solution, then stir for 15min at -78°C; then Stir at 0°C for 1h; then add allyl bromide (0.72g) and anhydrous tetrahydrofuran (15mL) to the mixed solution, then stir for 12h at a temperature of 25°C; then add methanol ( 5mL), then vacuum dried to obtain the crude product; then the crude product was dissolved in dichloromethane, and washed with deionized water, brine, MgSO 4 The solid was dried, and finally the oily substance 4-(3-butenyl)-4'-methyl-2,2'-bipyridine was obtained by column chromatography; then 4-(3-butenyl)-4' -Methyl-2,2'-bipyr (0.0986g), chlorotetrakis[2-(2-pyridyl)phenyl]diiridium(III)(0.214g), ethylene glyc...

Embodiment 3

[0063] Embodiment 3: the preparation of mesoporous iridium pyridine catalyst (MCF-Ir):

[0064] First iridium pyridine catalyst (0.0500g), SH-MCF (0.1000g), AIBN (0.0200g) CHCl 3 (10mL) were mixed, and then refluxed in a nitrogen atmosphere for 24h; finally filtered, washed, and dried (80°C) to obtain a mesoporous iridium pyridine heterogeneous catalyst.

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Abstract

The invention discloses a meso-porous iridium pyridine heterogeneous catalyst, and a preparation method and an application thereof. The meso-porous iridium pyridine heterogeneous catalyst comprises a mercapto functionalized meso-porous foam silicon oxide matrix and an iridium pyridine catalyst covalently combined with the matrix, and active sites of the iridium pyridine catalyst are dispersed in the meso-porous tunnels of the matrix. The heterogeneous catalyst has a three dimensional tunnel structure. The preparation method of the heterogeneous catalyst is realized through a click chemical method, the heterogeneous catalyst can be well dispersed in a reaction system, grafted Ir<3+> active sides are dispersed on the inner walls of the pores of the heterogeneous catalyst, and the grafted Ir<3+> active sides are in mutually independent contact with a substrate, so the catalysis effect is realized, and mutual influences are avoided; the catalyst has good chemical and thermal stability, can eliminate reaction substrate diffusion influences, can be widely applied in photoinduced electron transfer reactions, and can be repeatedly used; and the preparation method has the advantages of simplicity, wide sources of raw materials, convenient and controllable operation, low cost, and easy large-scale enforcement.

Description

technical field [0001] The invention relates to a heterogeneous catalyst and its preparation process, in particular to a mesoporous iridium pyridine heterogeneous catalyst, its preparation method and application. Background technique [0002] Light energy is a non-toxic and non-polluting renewable energy. In recent years, the use of visible light for photocatalytic organic synthesis has become a hot topic and a foreword in organic chemistry research. As a typical visible light photosensitizer, the iridium complex photocatalyst changes from the ground state to the excited state after being excited by visible light in the process of photocatalytic organic synthesis, and reacts with reducing or oxidizing reaction substrates to realize the interaction between organic substrates. The single electron transfer process (SET). At present, the catalyst has been used in various light-induced organic synthesis systems. However, the existing homogeneous catalysts have disadvantages suc...

Claims

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Application Information

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IPC IPC(8): B01J31/22
Inventor 张昉郝中凯毛展
Owner SHANGHAI NORMAL UNIVERSITY
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