Heterogeneous catalysts for alkene hydroformylation reaction and preparation method thereof

A technology of olefin hydroformyl and catalyst, which is applied in the field of preparation of supported metal catalysts, can solve problems such as loss of ligands, loss of ligands and metals, lack of coordination effect, etc., and achieve the effect of improving activity

Active Publication Date: 2014-01-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to solve the ligand loss problem of the above two catalysts, CN 1016427219A discloses an anchoring ligand-modified supported metal catalyst and its preparation method and application. The organic ligands and metal components on the catalyst are directly fixed to the carrier At the same time, there is a coordination between the organic ligand and the metal component to generate active species in situ. This catalyst can solve the problem of ligand and metal loss, but since both the ligand and the metal are anchored on the support, it cannot Free movement, many ligands cannot effectively contact with metal atoms, no coordination effect, and the activity of the catalyst is very low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 5.0g of silica gel, cook for 10 hours, dry at 393K, and set aside. RhCl with a Rh content of 1wt% was prepared separately 3 10.0ml of aqueous solution and Al(NO 3 ) 3 10.0ml aqueous solution, impregnated the above silica gel with these two aqueous solutions at the same time, baked in an oven at 393K for 12 hours after natural drying, then baked in a muffle furnace at 573K for 4 hours, and finally heated it with H at 393K 2 After 4 hours of reduction, 1Rh1Al / SiO with both Rh loading and Al loading at 1wt% was obtained 2 catalyst.

[0032] Take 0.034g of 2-(diphenylphosphine)propyltriethoxysilane and dissolve it in 3.0ml of toluene. Add 0.30g of 1Rh1Al / SiO prepared above 2 catalyst, and then the mixture was stirred at room temperature for 15 hours, and then stirred at reflux for 6 hours in a 383K oil bath. Finally, the refluxed mixture was naturally cooled to room temperature and the solvent was vacuum-extracted at room temperature to obtain DPPPTS-1Rh1Al / SiO ...

Embodiment 2

[0034] Take 5.0g of silica gel, cook for 10 hours, dry at 393K, and set aside. RhCl with a Rh content of 1wt% was prepared separately 3 Aqueous solution 10.0ml and AgNO with Ag content 1wt% 3 10.0ml aqueous solution, impregnated the above silica gel with these two aqueous solutions at the same time, baked in an oven at 393K for 12 hours after natural drying, then baked in a muffle furnace at 573K for 4 hours, and finally heated it with H at 393K 2 After reduction for 4 hours, 1Rh1Ag / SiO with both Rh loading and Ag loading at 1wt% was obtained 2 catalyst.

[0035] Take 0.034g of 2-(diphenylphosphine)propyltriethoxysilane and dissolve it in 3.0ml of toluene. Add 0.30g of 1Rh1Ag / SiO prepared above 2 catalyst, and then the mixture was stirred at room temperature for 15 hours, and then stirred at reflux for 6 hours in a 383K oil bath. Finally, the refluxed mixture was naturally cooled to room temperature and the solvent was vacuum-extracted at room temperature to obtain DPPPTS...

Embodiment 3

[0037] Take 5.0g of silica gel, cook for 10 hours, dry at 393K, and set aside. RhCl with a Rh content of 1wt% was prepared separately 3 Aqueous solution 10.0ml and CuCl with Cu content 1wt% 2 10.0ml aqueous solution, impregnated the above silica gel with these two aqueous solutions at the same time, baked in an oven at 393K for 12 hours after natural drying, then baked in a muffle furnace at 573K for 4 hours, and finally heated it with H at 393K 2 After 4 hours of reduction, 1Rh1Cu / SiO with both Rh loading and Cu loading at 1wt% was obtained 2 catalyst.

[0038] Take 0.034g of 2-(diphenylphosphine)propyltriethoxysilane and dissolve it in 3.0ml of tetrahydrofuran. Add 0.30g of 1Rh1Cu / SiO prepared above 2 catalyst, and then the mixture was stirred at room temperature for 15 hours, and then stirred at reflux for 6 hours in a 383K oil bath. Finally, the refluxed mixture was naturally cooled to room temperature and the solvent was vacuum-extracted at room temperature to obtain...

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Abstract

The invention discloses a supported metal catalyst under double modification of an anchoring ligand and an auxiliary and a preparation method and application thereof. The catalyst comprises an active component, an auxiliary, a carrier and a ligand, wherein the active component is one or more of metals Rh, Ru and Co; the auxiliary is one or more of Al, K, Zn, Cu and Ag; the carrier is a molecular sieve SiO2, Al2O3, MCM-41 or SBA-15; the ligand is an N or P-containing organic ligand capable of acting with silicon hydroxyl. In the catalyst, the metal component and the auxiliary are directly fixed on the carrier, and then the anchoring ligand and the metal generate a coordination action to in-situ generate an active species; due to the double modification of the ligand and the auxiliary, the activity and stability of the catalyst are remarkably improved. The catalyst can be applied to alkene hydroformylation to prepare various organic aldehydes, has relatively high catalytic activity and excellent stability, and is easy to separate.

Description

technical field [0001] The invention relates to a preparation method of a supported metal catalyst applied to olefin hydroformylation reaction, and the catalyst is a heterogeneous metal catalyst double-modified by a ligand and an auxiliary agent. Background technique [0002] Since the German scientist Otto Roelen discovered the hydroformylation reaction in the Ruhrchemie laboratory in Oberhausen in 1938, and soon built the first industrial device in the early 1940s, the research on the hydroformylation reaction of olefins has been prosperous for a long time. . The reason why hydroformylation technology has become one of the most important petrochemical technologies is mainly because its product aldehyde is a very useful chemical intermediate, which can synthesize carboxylic acids and their corresponding esters, as well as fatty amines, etc., the most important The purpose is that it can be converted into alcohol by hydrogenation, and alcohol itself can be widely used in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/24B01J31/22C07C47/02C07C45/50
Inventor 严丽刘佳丁云杰朱何俊姜淼
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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