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Preparation and application of amphiphilic magnetic palladium-loaded nano-ferric oxide and emulsion thereof

A magnetic nano, palladium nano technology, applied in metal/metal oxide/metal hydroxide catalysts, organic chemistry, hydrocarbons, etc., can solve incomplete separation of surfactants, limit the application of surfactant aggregates, Catalyst recovery and reuse is difficult to achieve the effect of efficiently catalyzing the Suzuki reaction, simplifying demulsification separation and catalyst recovery

Inactive Publication Date: 2012-07-04
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Similar to phase transfer catalysis, emulsions generally have problems such as incomplete separation of surfactants from products, difficulties in the recovery and reuse of emulsion components and catalysts in organic synthesis, which severely limit the use of emulsions and other surfactant aggregates in organic synthesis. Applications

Method used

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  • Preparation and application of amphiphilic magnetic palladium-loaded nano-ferric oxide and emulsion thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The present embodiment follows the steps: the magnetic nano-Fe 3 o 4 The particles are placed in deionized water, the concentration of solid particles is 5-50g / L, the pH of the solution is adjusted to 4-6, and n-octyl acid is added under stirring. The amount of n-octyl acid is Fe 3 o 4 10%-50% of the particles, adjust the pH of the solution to 7 after reacting for 30-60 minutes, and separate Fe with a magnet 3 o 4 Wash the particles with ethanol for 2-3 times, and dry to obtain amphiphilic magnetic nano-Fe 3 o 4 Particles; put the particles into Na with a concentration of 3-10mmol / L 2 PdCl 4 In aqueous solution, control Fe 3 o 4 The mass ratio of particles to palladium is 1-10%, hydrogen gas is introduced under stirring, and Fe is separated with a magnet after the end 3 o 4 particles, to obtain amphiphilic palladium-loaded magnetic nano-Fe 3 o 4 particles, attached figure 1 TEM image of the particle.

[0021] Take 0.1-1.5g amphiphilic palladium-loaded magn...

Embodiment 2

[0023] This embodiment prepares amphiphilic loaded palladium magnetic nano-Fe 3 o 4 Particle is the same as embodiment 1, gets 0.1-1.5g loaded palladium amphiphilic magnetic nanometer Fe 3 o 4 Particles were added to 10 mL of n-heptane / water (n-heptane to water volume ratio 1:1) solution, and emulsified with a high-shear emulsifier at 5000 rpm for 3-10 minutes to obtain a water-in-oil type ( W / O) Pickering Lotion. Solubilize 10mmol bromobenzene, 10mmol phenylboronic acid and 15mmol NaOH in the Pickering emulsion, react at 80°C for 2 hours, and separate Fe with a magnet after the reaction 3 o 4 Particles and emulsions are automatically divided into two phases of oil and water, and the product is collected in the oil phase with a yield of 82%. Palladium-loaded amphiphilic magnetic nano-Fe 3 o 4 The particles were washed with deionized water and ethanol and reused.

Embodiment 3

[0025] The present embodiment follows the steps: the magnetic nano-Fe 3 o 4 The particles are placed in deionized water, the concentration of solid particles is 5-50g / L, the pH of the solution is adjusted to 4-6, and n-hexyl acid is added under stirring. The amount of n-hexyl acid is Fe 3 o 4 10%-50% of the particles, adjust the pH of the solution to 7 after reacting for 30-60 minutes, and separate Fe with a magnet 3 o 4 Wash the particles with ethanol for 2-3 times, and dry to obtain amphiphilic magnetic nano-Fe 3o 4 Particles; put the particles into Na with a concentration of 3-10mmol / L 2 PdCl 4 In aqueous solution, control Fe 3 o 4 The mass ratio of particles to palladium is 1-10%, and 2-10mmol / L NaBH is added under stirring 4 Aqueous solution 10mL, after the end, use a magnet to separate Fe 3 o 4 particles, to obtain amphiphilic palladium-loaded magnetic nano-Fe 3 o 4 particle.

[0026] In this embodiment, the steps of preparing Pickering emulsion and catalyz...

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Abstract

The invention discloses a preparation method of a Pickering emulsion by utilizing amphiphilic magnetic palladium-loaded nano Fe3O4 particles, and a method of carrying out an organic synthetic reaction in the Pickering emulsion. The preparation method is characterized by comprising the following steps: modifying nano Fe3O4 particles by using alkyl carboxylic acid and salts thereof to enable the particles to have amphiphilic property; loading palladium to the particles, thus preparing amphiphilic palladium-loaded nano FeO4 particles with catalytic activity; preparing the Pickering emulsion in oil-water phase, and applying the Pickering emulsion to a Suzuki reaction; adsorbing all magnetic nano-particles by using a magnet after the reaction is completed; and automatically separating the emulsion into an oil phase and a water phase to facilitate the separation and reclamation of a catalyst. According to the preparation method, a complicated process of removing a surfactant in a conventional emulsion is avoided, and a process of reclaiming nano-particles by adopting a filter mode is avoided, so that breaking emulsion separation, catalyst reclamation and other operations are simplified.

Description

technical field [0001] The invention relates to a kind of palladium-supported nano-Fe with amphiphilic 3 o 4 Particle preparation method, especially the method of preparing Pickering emulsion by using the amphiphilic palladium nano-catalyst particles, and the application of the Pickering emulsion in organic synthesis. Background technique [0002] Emulsions represent an important class of self-assembled amphiphilic systems, which are dispersion systems formed by two immiscible liquids (such as oil and water) under the action of surfactant molecular interface film. Emulsions have been widely studied in the fields of detergents, fuels, extraction, environmental protection, organic synthesis, polymer chemistry, biochemistry, and nanomaterial preparation. [0003] Similar to phase transfer catalysis, in the organic synthesis of emulsions, there are generally problems such as incomplete separation of surfactants from products, difficulties in the recovery and reuse of emulsion ...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C15/14C07C1/32
Inventor 蒋建中崔哲万乐平李解崔正刚
Owner JIANGNAN UNIV
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