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A method for preparing nanoscale spherical phenolic resin-loaded gold composite particles

A technology of phenolic resin and composite particles, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of reduced catalytic activity, less deposition, catalyst poisoning, etc., and achieves high catalytic activity without reduction. agent, the effect of high loading rate

Inactive Publication Date: 2015-11-04
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Bare gold nanoparticles are easily matured and aggregated, which leads to their inactivation during the catalytic reaction process. Since gold nanoparticles are easily adsorbed with reactants and products during the catalytic process, the catalyst is poisoned and its catalytic activity is also reduced. greatly reduce, or even inactivate
[0004] Currently, the methods for preparing supported gold nanocatalysts mainly include the following: 1. Impregnation method, adding oxide carriers such as silicon oxide, aluminum oxide, and magnesium oxide to a gold source (chloroauric acid, gold chloride, etc.) In the solution, through heat treatment afterwards, obtain supported type gold nano catalyst, but the particle size of gold is all very big, and deposition amount is also less; The co-precipitate is obtained in the mixed solution of salt, and then washed with water, dried, and roasted in the air to obtain the corresponding gold catalyst. This method is simple, but the disadvantage is that some gold particles will be buried in the carrier.

Method used

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  • A method for preparing nanoscale spherical phenolic resin-loaded gold composite particles
  • A method for preparing nanoscale spherical phenolic resin-loaded gold composite particles
  • A method for preparing nanoscale spherical phenolic resin-loaded gold composite particles

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: Preparation of phenolic resin nano-spherical template

[0022] Add 0.2 mol of phenolic substances (resorcinol, phenol, 4-aminophenol), 0.1 mol of formaldehyde, and 200 microliters of ammonia solution with a mass fraction of 25% to 28 mL of alcohol-water mixed solution (the ratio of ethanol volume to water volume 2:5), heated at 30°C for 3h, and then put the above mixture into a closed reaction kettle and cured at 160°C for 6h to obtain a phenolic resin nanosphere template with a size of 200nm.

[0023] The phenolic resin spherical nanoparticle transmission electron microscope photograph that the present embodiment prepares sees figure 1 .

Embodiment 2

[0024] Embodiment 2: impregnation method carries out the loading of small gold particles (1)

[0025] The phenolic resin spherical nano-template (prepared from resorcinol) particles in Example 1 were dispersed into the aqueous solution, and the concentration was adjusted to 8 mg / mL. Add different volumes (50 μL, 100 μL, 200 μL, 300 μL, 400 μL, 500 μL) of chloroauric acid aqueous solution (27 mM) into 9 mL of water, and then add different volumes of water again, so that the volume of the entire system is 10 mL. Keep it in the dark for one hour, add 1 mL of phenolic resin solution, react at room temperature for 15 minutes, and centrifuge to obtain the final product. The sizes of the obtained small gold particles are 3.2, 3.7, 4.2, 5.5, 6.7, and 8.3 nm. 3%, 6%, 12%, 18%, 24%, 33%, washed 3 to 5 times.

[0026] The particle diameters of the phenolic resin spherical nanoparticles loaded by the present embodiment are 3.7nm, 4.2nm, 5.5nm gold particles, and the catalytic rate reacti...

Embodiment 3

[0027] Example 3: Loading of small gold particles by impregnation method (2)

[0028] The phenolic resin spherical nano-template (prepared from resorcinol) particles in Example 1 were dispersed into the aqueous solution, and the concentration was adjusted to 8 mg / mL. 500 μL of 27 mM chloroauric acid aqueous solution was added to 9 mL of water, and then water was added again, so that the volume of the whole system was 10 mL. Adjust the pH value of the system to 2 or 2.5, keep it in the dark for one hour, add 1 mL of phenolic resin solution, react at room temperature for 15 minutes, and centrifuge to obtain the final product. The size of the obtained small gold particles is 4.3nm, and the gold loading capacity 33%, washed 3 to 5 times.

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Abstract

The invention discloses a method for preparing nanoscale phenolic resin gold-loaded composite particles and belongs to the technical field of functional nanoparticles. The preparation process comprises the following steps: preparing a chloroauric acid solution, and preserving the solution for an hour in a shaded mode; dispersing a phenolic resin nanometer spherical template in water, so as to obtain a phenolic resin nanometer spherical template dispersion; mixing the mixed chloroauric acid solution and the phenolic resin nanometer spherical template dispersion according to a certain volume ratio, regulating the pH to be 2-6, reacting at the temperature of 20-60 DEG C for 1-15 minutes, and centrifuging to obtain the nanoscale phenolic resin gold-loaded composite particles. The gold loading capacity is 3-33 percent, the particle size of the gold particles is 3-8.5nm, and the gold particles can serve as a loaded gold particle catalyst. The method is simple in preparation and high in reproducibility, and a reducing agent is not needed. Moreover, the nanoscale phenolic resin gold-loaded composite particles have the high load rate and the high catalytic activity.

Description

technical field [0001] The invention belongs to the technical field of functional nanoparticles, in particular to a supported gold nanoparticle catalyst and a preparation method thereof. Background technique [0002] Supported gold nanoparticles are widely used as catalysts in many fields. Due to its size effect, gold nanoparticles have a very wide range of applications, especially in the field of organic catalysis, such as low-temperature oxidation of carbon monoxide, catalytic combustion of hydrocarbons, and selective hydrogenation of unsaturated hydrocarbons. [0003] Bare gold nanoparticles are easily matured and aggregated, which leads to their inactivation during the catalytic reaction process. Since gold nanoparticles are easily adsorbed with reactants and products during the catalytic process, the catalyst is poisoned and its catalytic activity is also reduced. greatly reduced, or even inactivated. [0004] Currently, the methods for preparing supported gold nanoca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06C07C209/36C07C211/46
Inventor 杨文胜郑维时庄家骐郭子龙
Owner JILIN UNIV