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A method for preparing amino compounds by catalytically reducing aromatic nitro compounds with high efficiency

A technology of amino compounds and aromatic nitro groups, applied in the field of reduction of aromatic nitro compounds, can solve problems such as slow catalytic rate of catalysts

Inactive Publication Date: 2017-08-25
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, gold, silver and their gold-silver alloy nano-catalysts are commonly used, but the catalytic rate of the above-mentioned catalysts is slow. Therefore, it is urgent to develop a more efficient catalyst.

Method used

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  • A method for preparing amino compounds by catalytically reducing aromatic nitro compounds with high efficiency
  • A method for preparing amino compounds by catalytically reducing aromatic nitro compounds with high efficiency
  • A method for preparing amino compounds by catalytically reducing aromatic nitro compounds with high efficiency

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Press Ru 3+ : PVP monomer molar ratio is 1:10, weigh a certain amount of RuCl 3 ·nH 2 O and PVP, fully dissolve them in 10 ml of n-propanol under ultrasound, pour the above mixed solution into a 50 ml round bottom flask, add a stirring bar, stir rapidly at room temperature in a water bath for 10 hours, the solution turns from brownish red to final Turned brown, that is, the reaction is complete. Mix the original solution with the precipitating agent acetone 1:3 and then centrifuge. After centrifuging at 8000 rpm for 5 minutes, take the precipitate and wash it with water. Repeatedly washing with acetone and deionized water for 3-5 times, the obtained precipitate is dissolved in water to become an aqueous solution of ruthenium nanoparticles.

[0026] Add 2 ml of 0.1 mol / L freshly prepared sodium borohydride solution and 10 μL of 10 -2 mol / liter prepared p-nitrophenol aqueous solution, and finally add a small amount of synthesized ruthenium nanoparticle aqueous solutio...

Embodiment 2

[0028] Press Ru 3+ : PVP monomer molar ratio is 1:10, weigh a certain amount of RuCl 3 ·nH 2 O and PVP, fully dissolve them in 10 ml of n-propanol under ultrasound, pour the above mixed solution into a 50 ml round bottom flask, add a stirring bar, stir rapidly at room temperature in a water bath for 10 hours, the solution turns from brownish red to final Turned brown, that is, the reaction is complete. Mix the original solution with the precipitating agent acetone 1:3 and then centrifuge. After centrifuging at 8000 rpm for 5 minutes, take the precipitate and wash it with water. Repeatedly washing with acetone and deionized water for 3-5 times, the obtained precipitate is dissolved in water to become an aqueous solution of ruthenium nanoparticles.

[0029] Add 2 ml of 0.1 mol / L freshly prepared sodium borohydride solution and 10 μL of 10 -2 mol / liter prepared p-nitroaniline ammonia solution, and finally add a small amount of synthesized ruthenium nanoparticle aqueous soluti...

Embodiment 3

[0031] Press Ru 3+ : PVP monomer molar ratio is 1:10, weigh a certain amount of RuCl 3 ·nH 2 O and PVP, fully dissolve them in 10 ml of n-propanol under ultrasound, pour the above mixed solution into a 50 ml round bottom flask, add a stirring bar, stir rapidly at room temperature in a water bath for 10 hours, the solution turns from brownish red to final Turned brown, that is, the reaction is complete. Mix the original solution with the precipitating agent acetone 1:3 and then centrifuge. After centrifuging at 8000 rpm for 5 minutes, take the precipitate and wash it with water. Repeatedly washing with acetone and deionized water for 3-5 times, the obtained precipitate is dissolved in water to become an aqueous solution of ruthenium nanoparticles.

[0032] Add 2 ml of 0.1 mol / L freshly prepared sodium borohydride solution and 10 μL of 10 -2 mol / liter prepared p-chloronitrobenzene aqueous solution, and finally add a small amount of synthesized ruthenium nanoparticle aqueous ...

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Abstract

The invention provides a method efficiently catalytically reducing aromatic nitro compounds to prepare amino compounds. The method has the advantages that the method is applicable to the catalytic reduction of all aromatic nitro compounds, the catalyzing speed of the method is much higher than that of other metal nano catalysts, and the catalyzing speed of the method is more than ten times even dozens of times of that of gold and silver and gold-silver-alloy nano particles; the catalyzing reaction is high in catalyzing activity, high in adaptability, mild in reaction condition, simple to operate, practicable and promising in application prospect.

Description

technical field [0001] The invention relates to the reduction of aromatic nitro compounds, in particular to the research on the catalytic reduction of aromatic nitro compounds using ruthenium nanoparticles as a catalyst, and belongs to the field of catalytic reduction. Background technique [0002] Aromatic amino compounds are widely used in chemical, pharmaceutical, pesticide, dye and other fields, and are important intermediates in organic synthesis. The synthesis of aromatic amino compounds is generally obtained by reducing the corresponding aromatic nitro compounds as raw materials, mainly including iron filings reduction method, electrochemical method, and catalytic hydrogenation method. [0003] Although the iron filings reduction method is basically applicable to the reduction of all nitro compounds, and the operating conditions are mild, the produced arylamine-containing iron sludge and waste water have serious environmental pollution problems. Therefore, this metho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/02C07C215/76C07C215/80C07C209/36C07C211/52C07C211/51C07C227/04C07C229/60B01J23/46
CPCB01J23/462B01J35/0013C07C209/36C07C213/02C07C227/04C07C215/76C07C215/80C07C211/52C07C211/51C07C229/60
Inventor 赵媛宋启军罗耀东杨璇
Owner JIANGNAN UNIV
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