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Mesoporous carbon-loaded gold nano catalyst and application thereof

A gold nanometer and mesoporous carbon technology, which is applied in organic chemistry, amino compound preparation, chemical instruments and methods, etc., can solve the problem of poor oxidation activity of cyclohexene, achieve high specific surface area, no environmental pollution, and simple operation process easy effect

Active Publication Date: 2013-11-13
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the particle size of Au reaches 6-7nm, and the corresponding cyclohexene oxidation activity is not as good as that of Au / SBA-15 (Fatme kerdi, Valerie Caps, Alain Tuel.Micropor.Mesopor.Mater, 2011, 140:89-96)

Method used

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  • Mesoporous carbon-loaded gold nano catalyst and application thereof
  • Mesoporous carbon-loaded gold nano catalyst and application thereof
  • Mesoporous carbon-loaded gold nano catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: the preparation of Au / SBA-15

[0042] (1) SBA-15-NH 4 + Preparation: 1.0g SBA-15 (prepared according to the literature report of Zhao Dongyuan’s research group, Dongyuan Zhao, Jinyu Sun, Quanzhi Li, Galen D.Stucky.Chem.Mater.2000, 12:275-279.), 2g γ- Add aminopropyltriethoxysilane and 120g ethanol into a 250ml one-necked flask, and heat to reflux for 12h. After cooling, filter, wash with ethanol three times, and dry at room temperature for 12 hours.

[0043] (2) Loading reaction of Au: take 2.5ml chloroauric acid solution (0.02g / ml), dilute to 20ml, and mix with 1.0gSBA-15-NH 4 + Mix and stir at room temperature for 30 min. Weigh 0.1gKBH 4 , Prepare a solution with 10ml of distilled water, add it dropwise to the above mixture, and continue to stir for 1h. Filter, wash with water and ethanol, and dry at room temperature for 10 h. The obtained sample is characterized by X-ray diffraction, transmission electron microscopy and nitrogen gas adsorption, ...

Embodiment 2

[0044] Embodiment 2: Preparation of Au / mesoporous carbon

[0045] Get the Au / SBA-15 that 1.0g embodiment 1 makes in watch glass, then take by weighing 4.0g 25% phenolic resin (prepared by the method described in literature Joo, S.H.; Choi, S.J.; Oh, I.; Kwak , J.; Liu, Z.; Terasaki, O.; Ryoo, R.Nature 2001, 412 (6843), 169.) solution was added to the same watch glass, after stirring evenly, soaked for 2 hours. After drying in air for 5 hours, transfer into quartz boats. Put the quartz boat into a quartz tube furnace, and program the temperature rise carbonization under the protection of nitrogen. The setting of the temperature program is: increase the temperature to 350°C at a rate of 1°C / min, maintain at 350°C for 2 hours, continue to increase the temperature to 700°C at a rate of 1°C / min, and maintain for 2 hours. Weigh 50g of ethanol, 2g of NaOH, and 40g of water to prepare lye. Transfer the carbonized sample and lye into a polytetrafluoroethylene tube, and keep the reac...

Embodiment 3

[0046] Example 3: Activity Evaluation of Au / Mesoporous Carbon Catalyzed O-Chloronitrobenzene Hydrogenation

[0047] In a 100ml stainless steel autoclave, add 0.1g of Au / mesoporous carbon prepared in Example 2, 5.0g of o-chloronitrobenzene, and 50ml of ethanol. Seal the reaction kettle, replace the air in the kettle with nitrogen, raise the temperature to 130°C, add hydrogen to 3Mpa, start stirring (1000r / min), react at constant temperature for 7 hours, stop the reaction and cool to room temperature. The reaction solution was taken out, the catalyst was removed by filtration, and the filtrate was analyzed by gas chromatography. The conversion rate of o-chloronitrobenzene was 94.3%, the selectivity of o-chloroaniline was 98.3%, and the dechlorination was only 0.3%.

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Abstract

The invention discloses a mesoporous carbon-loaded gold nano catalyst and application of the catalyst. A preparation method of the mesoporous carbon-loaded gold nano catalyst comprises the following steps of: (1) mixing SBA-15, gamma-aminopropyltriethoxysilane and ethanol, refluxing for 8-10h, filtering and drying to obtain amino-modified SBA-15; (2) mixing amino-modified SBA-15 with HAuCl4 aqueous solution, sufficiently stirring, and then adding KBH4 aqueous solution for reduction to obtain Au / SBA-15; and (3) uniformly mixing Au / SBA-15 obtained in the step (2) with phenolic resin ethanol solution, sufficiently immersing, carrying out primary drying, then transferring to a pipe furnace, carrying out high-temperature carbonization in nitrogen atmosphere at 600-900 DEG C, taking out obtained solid, and washing off the template SBA-15 to obtain the mesoporous carbon-loaded gold nano catalyst. The obtained mesoporous carbon-loaded gold nano catalyst can be used for hydrogenation reaction of nitrobenzene compounds, and has excellent reaction activity and selectivity.

Description

(1) Technical field [0001] The invention belongs to the technical field of noble metal catalysis, relates to a mesoporous carbon-supported gold nano-catalyst, and applies it to the reaction of preparing aniline compounds by catalytic hydrogenation of nitrobenzene compounds. (2) Background technology [0002] Mesoporous carbon materials have been widely used in the fields of adsorption and separation, catalysis, and conductive materials due to their unique structural properties, such as high specific surface area, uniform distribution of mesoporous channels, better hydrothermal stability, and chemical inertness. In the field of catalysis, mesoporous carbon has been proved to be an excellent catalyst support. So far, there have been a lot of reports about the preparation and application of mesoporous carbon-supported metal catalysts to catalyze organic reactions. With mesoporous carbon materials CMK-1 and CMK-3 as carriers, H 2 PtCl 6 , RuCl 3 ·H 2 O, Pd(NO 3 ) 2 and ot...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/52C07C209/36C07C211/52C07C211/47C07C211/46C07C213/02C07C217/84
Inventor 严新焕顾辉子
Owner ZHEJIANG UNIV OF TECH
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