A kind of high-efficiency nano-gold-based catalytic hydrogenation catalyst and preparation method thereof

A hydrogenation catalyst and catalytic hydrogenation technology, applied in the preparation of amino compounds, amino hydroxyl compounds, physical/chemical process catalysts, etc., can solve the problems of nano-gold loss, unfavorable catalyst recycling, etc.

Inactive Publication Date: 2011-12-14
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the gold nanoparticles loaded on the surface will be lost with the progress of the reaction, which is not conducive to the recycling of the catalyst.

Method used

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  • A kind of high-efficiency nano-gold-based catalytic hydrogenation catalyst and preparation method thereof
  • A kind of high-efficiency nano-gold-based catalytic hydrogenation catalyst and preparation method thereof
  • A kind of high-efficiency nano-gold-based catalytic hydrogenation catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 10g 58 was dissolved in 50 mL of cyclohexane, stirred and heated to 50 °C and completely dissolved. Take 1.5mL of chloroauric acid with a concentration of 0.5mol / L, add hydroxyethylethylenediamine, until the chloroauric acid solution changes from cloudy to uniform and transparent again, then add it into the surfactant system, stir and disperse until the whole system is uniform transparent. Insulate and stir until the color of the system becomes lighter, add 0.1g of sodium borohydride, add 0.1mL of mercaptoethanol after the gold ions are completely reduced, stir until the system is uniform and transparent, adjust the pH of the reaction solution to 10.5-11 with ammonia water, drop into Tetraethyl orthosilicate 10g, stirred and reacted for 2h. After centrifugation, washing, drying, roasting, and reduction, electron microscope observation is carried out, such as figure 1 shown; characterized by high-angle annular dark field-scanning transmission electron microscopy ( ...

Embodiment 2

[0029] Dissolve 12g of Triton X-100 in 50mL of cyclohexane, stir and heat to 50°C and dissolve completely. Take 1.5mL of chloroauric acid with a concentration of 0.5mol / L, add hydroxyethylethylenediamine, until the chloroauric acid solution changes from cloudy to uniform and transparent again, then add it into the surfactant system, stir and disperse until the whole system is uniform transparent. Insulate and stir until the color of the system becomes lighter, add 0.1g of sodium borohydride, add 0.1mL of mercaptoethanol after the gold ions are completely reduced, stir until the system is uniform and transparent, adjust the pH of the reaction solution to 10.5-11 with ammonia water, drop into Tetraethyl orthosilicate 10g, stirred and reacted for 2h. After centrifugation, washing, drying, roasting, and reduction, electron microscope observation is carried out, such as image 3 As shown, the product is in the shape of a strip, the cavity diameter is 8-10nm, the aspect ratio is 2...

Embodiment 3

[0031] 10g 58 was dissolved in 50 mL of cyclohexane, stirred and heated to 50 °C and completely dissolved. Take 1.5mL of chloroauric acid with a concentration of 0.5mol / L, add hydroxyethylethylenediamine, until the chloroauric acid solution changes from cloudy to uniform and transparent again, then add it into the surfactant system, stir and disperse until the whole system is uniform transparent. Insulate and stir until the color of the system becomes lighter, add 0.1g of sodium borohydride, add 0.1mL of mercaptoethanol after the gold ions are completely reduced, stir until the system is uniform and transparent, adjust the pH of the reaction solution to 10.5-11 with ammonia water, drop into Tetraethyl orthosilicate 10g, stirred and reacted for 2h. After centrifugation, washing, drying, roasting, reduction, and electron microscope observation, the product particles are uniform, the particle diameter is 40-50nm, the nanometer metal particle diameter is less than 2nm, and the ...

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Abstract

A high-efficiency nano-gold-based hydrogenation catalyst and a preparation method thereof belong to the technical field of preparation of a nano-gold-based catalyst with high catalytic activity and high selectivity. In the preparation method, a mixed solution of chloroauric acid and a bifunctional complexing agent is added to a uniform reverse micelle system under stirring conditions, followed by adding a reducing agent, then adding a bifunctional gold cluster complexing agent, and then adding alkali and silicic acid ester, and a highly efficient catalyst in which gold nanoclusters are dispersed in the porous structure of silica is obtained after stirring reaction. This catalyst can efficiently catalyze the hydrogenation reduction of aromatic nitro compounds to corresponding aromatic amines. In the presence of hydrazine hydrate, sodium borohydride and isopropanol, aromatic nitro compounds can be reduced to the corresponding aromatic amines under mild reaction conditions.

Description

technical field [0001] The invention relates to a high-efficiency nanometer gold-based hydrogenation catalyst and a preparation method thereof, belonging to the technical field of preparation of a nanometer gold-based catalyst with high catalytic activity and high selectivity. Background technique [0002] In recent years, people have found through systematic research on gold nanoparticles that they can catalyze reactions that are difficult for other metals to catalyze, and have high activity and specific selectivity. Corma et al. used titanium dioxide to support gold nanoparticles, which can efficiently catalyze the hydrogenation reduction of aromatic nitro compounds to the corresponding aromatic amines, and even specifically reduce the nitro group of aromatic nitro compounds containing olefinic double bonds and carbonyl groups. However, the gold nanoparticles supported on the surface will be lost with the progress of the reaction, which is not conducive to the recycling of...

Claims

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Application Information

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IPC IPC(8): B01J23/52B01J35/10C07B43/04C07C225/22C07C221/00C07C223/06C07C209/36C07C211/46C07C211/52C07C229/60C07C227/04C07C213/02C07C215/76C07C319/20C07C323/36C07C309/46C07C303/22
Inventor 吕荣文邹伟
Owner DALIAN UNIV OF TECH
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