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Preparation method of magnetic nano triphenylphosphine catalysis ligand

A magnetic nano and triphenylphosphine technology, applied in chemical instruments and methods, carbon monoxide reaction preparation, physical/chemical process catalysts, etc., to achieve the effects of improving catalytic activity, uniform size distribution, and improving catalytic efficiency

Inactive Publication Date: 2015-04-01
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, using dopamine as a coupling agent to immobilize triphenylphosphine ligands on the surface of magnetic nano-iron oxides to prepare magnetic nano-triphenylphosphine catalytic ligands has not been reported yet.

Method used

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  • Preparation method of magnetic nano triphenylphosphine catalysis ligand

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: the synthesis of ferric oleate

[0018] Synthesize iron oleate according to the method of T. Hyeon et al. (Nature Mater. 2004, 3, 891~895), the specific method is as follows: take 2.71 g FeCl 3 ·6H 2 O and 9.13 g of sodium oleate were mixed in a mixed solvent of 20 mL of ethanol, 15 mL of distilled water and 35 mL of n-hexane. The resulting mixture was stirred and reacted at 70 °C for 4 h, and the organic phase was separated, and the organic phase was washed with distilled water (3 ×10 mL), and then evaporated the solvent under reduced pressure with a rotary evaporator to obtain 9.12 g of dark brown viscous product iron (I) oleate.

Embodiment 2

[0019] Example 2: Preparation of Magnetic Nano Iron Oxide Particles by Thermal Decomposition

[0020] Refer to the method of T. Hyeon et al. (Nature Mater. 2004, 3, 891~895) to prepare magnetic nano-iron oxide particles. The specific method is as follows:

[0021] 9.12 g iron(I) oleate was dissolved in 41.1 g 1-octadecene and 1.17 g oleic acid was added, the resulting mixture was heated from room temperature to 340 °C at a rate of 3 °C / min and kept for 40 min, followed by the reaction The mixture was naturally cooled to room temperature to obtain a dark brown 1-octadecene solution of magnetic nano-iron oxide particles (II).

Embodiment 3

[0022] Embodiment 3: the pretreatment of magnetic nanometer iron oxide particle

[0023] Take 10 mL of 1-octadecene solution of magnetic nano-iron oxide particles (II), first wash with 95% ethanol (3×20 mL) to remove the solvent 1-octadecene, and then wash with 1:1 volume ratio of chloroform / Magnetic nano-iron oxide particles (3×10 mL) were washed with acetonitrile mixed solvent to remove excess oleic acid and irregular non-spherical nanoparticles to obtain relatively uniform magnetic nano-iron oxide particles (III) (diameter ~15 nm). The pretreated magnetic iron oxide nanoparticles (III) were stored in 5 mL chloroform until use.

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Abstract

The invention discloses a preparation method of a magnetic nano triphenylphosphine catalysis ligand, which comprises the following steps of: synthesizing magnetic nano iron oxide particles by a high-temperature pyrolysis method; removing the nano iron oxide particles with irregular appearance and redundant oleic acid on the surface by use of a chloroform / acetonitrile mixed solvent; synthesizing a triphenylphosphine dopamine derivative by taking 4-(diphenylphosphino)benzoic acid and dopamine as raw materials, and purifying through column chromatography; mixing the magnetic nano iron oxide particles and the triphenylphosphine dopamine derivative in DMF and performing ultrasonic stirring for 6 hours; sucking out the obtained magnetic nano triphenylphosphine ligand by a magnet; and washing the magnetic nano triphenylphosphine ligand with THF and storing in THF. The nano triphenylphosphine ligand prepared by the method can be applied to a catalytic hydroformylation reaction and can be sucked out by a magnet from a reaction mixture and repeatedly used.

Description

technical field [0001] The invention relates to a method for preparing a magnetic nano triphenylphosphine catalytic ligand, specifically a method for preparing magnetic nano triphenylphosphine by immobilizing triphenylphosphine dopamine derivatives on the surface of magnetic nano iron oxide particles through surface exchange reaction Ligand method. Background technique [0002] Triphenylphosphine is a homogeneous catalyst ligand widely used in the field of organic synthesis, which can form catalytically active complexes with various metals to catalyze corresponding organic chemical reactions. For example: triphenylphosphine and metal palladium catalyze Suzuki cross-coupling reaction (Angew. Chem. Int. Ed. 2001, 40, 4544~4568), and metal rhodium catalyze hydroformylation reaction (Coordin. Chem. Rev. . 1999, 190~192, 883~900), etc. Due to the good solubility of triphenylphosphine in various organic solvents, its separation, recovery and reuse from the catalytic reaction sys...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/24C07C45/50C07C47/228
Inventor 端木传嵩吴林林顾坚许兴友固旭冯良东
Owner HUAIYIN INSTITUTE OF TECHNOLOGY
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