Silicon dioxide supported nano-silver catalyst, preparation and use thereof

A silicon dioxide and catalyst technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, preparation of amino compounds, etc., can solve the problems of high cost, poor selectivity, inconvenient transportation, etc. The effect of reducing catalyst cost, mild reaction conditions and improving product quality

Inactive Publication Date: 2008-11-12
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 1. The metal powder-acid chemical reduction method produces a large amount of inorganic salt waste, which pollutes the environment and does not meet the requirements of green chemistry
Electrochemical reduction method has high requirements on electrodes, electrolyte and electrolytic cell, and is not suitable for mass production
[0005] 2. The catalysts used in the catalytic hydrogenation method are Raney nickel and platinum. During the production and use of Raney nickel catalysts, a large amount of alkaline wastewater is generated, and there are disadvantages such as difficult storage, inconvenient transportation, and poor reusability, especially product selectivity. Can not reach 100%, the generated by-products seriously affect product quality
Catalytic hydrogenation of nitroaromatic compounds with platinum catalyst is not only difficult to control the selectivity, but also requires precious platinum
Other noble metal catalysts are difficult to obtain in industry due to high cost and poor selectivity

Method used

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  • Silicon dioxide supported nano-silver catalyst, preparation and use thereof
  • Silicon dioxide supported nano-silver catalyst, preparation and use thereof
  • Silicon dioxide supported nano-silver catalyst, preparation and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] In the stainless steel reactor of 100ml, add 0.5 nitropyrene, 30ml ethanol and 0.10g catalyst 1# (Ag load capacity 1.0%), seal autoclave, fill H 2 Inflate to a pressure of 2.0MPa, then vent. Repeat the operation three times to remove the air in the kettle. Finally H 2 Charge to 2.0MPa, heat to 140°C, and react for 3.0 hours. During the reaction process, mechanical stirring was carried out at a speed of 900 revolutions per minute (900 r.p.m.). After the reaction was over, the reactor was naturally cooled to room temperature, and N 2 The gas is purged twice to remove the H in the kettle 2 . The catalyst is recovered from the reaction solution by centrifugation at a speed of 12000 r.p.m. The catalyst was washed three times with ethanol (3*5ml), and dried under vacuum at 60°C for recycling. The organic clear liquid was diluted with methanol and then analyzed and identified by GCMS-QP2010 (SHIMADZU) gas spectrometer. The results showed that the conversion rate of nitr...

Embodiment 2

[0033] In the stainless steel reactor of 100ml, add 0.5g nitropyrene, 30ml ethanol and 0.10g catalyst (Ag loading capacity 2.0%), seal autoclave, fill H 2 Inflate to a pressure of 2.0MPa, then vent. Repeat the operation three times to remove the air in the kettle. Finally H 2 Charge to 3.0MPa, heat to 140°C, and react for 3.0 hours. During the reaction process, mechanical stirring was carried out at a speed of 900 revolutions per minute (900 r.p.m.). After the reaction was over, the reactor was naturally cooled to room temperature, and N 2 The gas is purged twice to remove the H in the kettle 2 . The catalyst is recovered from the reaction solution by centrifugation at a speed of 12000 r.p.m. The catalyst was washed three times with ethanol (3*5ml), and dried under vacuum at 60°C for recycling. The organic clear liquid was diluted with methanol and then analyzed and identified by GCMS-QP2010 (SHIMADZU) gas spectrometer. The results showed that the conversion rate of nit...

Embodiment 3

[0035] In the stainless steel reactor of 100ml, add 0.5g nitropyrene, 30ml ethanol and 0.10g catalyst (Ag loading capacity 3.0%), seal autoclave, fill H 2 Inflate to a pressure of 2.0MPa, then vent. Repeat the operation three times to remove the air in the kettle. Finally H 2 Charge to 2.0MPa, heat to 140°C, and react for 3.0 hours. During the reaction process, mechanical stirring was carried out at a speed of 900 revolutions per minute (900 r.p.m.). After the reaction was over, the reactor was naturally cooled to room temperature, and N 2 The gas is purged twice to remove the H in the kettle 2 . The catalyst is recovered from the reaction solution by centrifugation at a speed of 12000 r.p.m. The catalyst was washed three times with ethanol (3*5ml), and dried under vacuum at 60°C for recycling. The organic clear liquid was diluted with methanol and then analyzed and identified by GCMS-QP2010 (SHIMADZU) gas spectrometer. The results showed that the conversion rate of nit...

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Abstract

The invention discloses a silicon dioxide load nanometer silver catalyst, preparation method and application in nitro compound catalytic hydrogenation reaction thereof. The preparing method comprises adding 1.0g of silicon dioxide in 20-50ml aqueous solution with 0.016g-0.064g of silver nitrate dissolved therein; stirring for 8-12 hours at 40 DEG C; adding 10-50ml of alcohol; heating up to 110 DEG C solvent thermal reaction for 8-12 hours; filtrating pale yellow solid; drying the solid at 100-120 DEG C for 8-12 hours to obtain the silicon dioxide load nanometer silver catalyst. The catalyst prepared by the invention is used for nitryl aromatic compound selective hydrogenation to prepare amido aromatic compound, and can realize complete transformation under optimization condition.

Description

technical field [0001] The invention relates to a silicon dioxide-supported nano-silver catalyst, a preparation method of the catalyst and its application in the selective hydrogenation of nitroaromatic compounds to prepare aminoaromatic compounds. Background technique [0002] Efficient and selective catalytic hydrogenation of aromatic nitro compounds is of great significance in the industrial field. Aminoaromatic compounds are very important chemical intermediates, which can be used to synthesize various fine chemicals such as pesticides, drugs, and photoelectric functional molecules. At present, the preparation methods of aminoaromatic compounds include: metal powder-acid chemical reduction method, electrochemical reduction method, and catalytic hydrogenation method. [0003] The main problems with these methods are: [0004] 1. The metal powder-acid chemical reduction method produces a large amount of inorganic salt waste, which pollutes the environment and does not me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/50B01J21/08C07C209/36
Inventor 薛伟李保军尹桂陈发胜
Owner NANJING UNIV
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