Catalyst in a highly active hydrogenation reaction of aromatic nitro compounds and preparation method thereof

An aromatic nitro, hydrogenation reaction technology, applied in the preparation of amino compounds, the preparation of organic compounds, the preparation of amino hydroxy compounds, etc., can solve problems such as very little graphene

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

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Problems solved by technology

[0005] However, most of the current research is on graphene nanoelectronic devices, such as electrodes, batteries, and supercapacitors, and few use graphene as a carrier for heterogeneous catalysis.

Method used

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  • Catalyst in a highly active hydrogenation reaction of aromatic nitro compounds and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0019] 1. The preparation process of graphene oxide (GO)

[0020] (1) Add 230 mL of 98% concentrated sulfuric acid into a 500 mL beaker, and control the temperature at 0°C;

[0021] (2) Add 10 g of graphite powder and 5 g of sodium nitrate, and stir for 1 h;

[0022] (3) Add 30 g of potassium permanganate powder under vigorous stirring, and control the temperature not to exceed 20°C during the addition process;

[0023] (4) Remove the low-temperature ice bath, and stir in a water bath at 35°C for 30 min;

[0024] (5) Add 460 mL of deionized water under stirring, raise the temperature of the reaction solution to about 98°C, and continue stirring for 1 h.;

[0025] (6) Dilute the reaction solution with 1.4 L deionized warm water, then add a certain amount of 3% hydrogen peroxide solution;

[0026] (7) Filtrate while hot, and wash the filter cake fully until there is no sulfate ion in the filtrate.

[0027] 2. Preparation process of graphene-supported Pt catalyst (Pt / RGO)

...

Embodiment 1

[0040] Take 0.02 g of catalyst and transfer it into the reaction kettle with 30 mL of ethanol. Put the reaction kettle into a water bath at 0°C, and stir for precooling for 1 h. After that, 1 mL of nitrobenzene was added quickly, and the reaction kettle was tightly closed. Check the airtightness of the reactor and fill it with hydrogen to 1 MPa. Then put the reaction kettle into a water bath at a set temperature, start stirring to 1000 rpm, and react for 180 min. After the set reaction time, stop the reaction. Take out the reaction solution in a 50 mL volumetric flask, add quantitative internal standard toluene, and make the volume to the mark. Then centrifuged, and the supernatant was taken for gas chromatography analysis. The results showed that the conversion rate of nitrobenzene was 100%, and the selectivity of aniline was 94.3%.

[0041]

Embodiment 2

[0043] Referring to the preparation method and steps of Example 1, the difference is that the reaction temperature was increased to 20°C, and the reaction time was shortened to 20 min. The results showed that the conversion rate of nitrobenzene was 100%, and the selectivity of aniline was 99.1%.

[0044]

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Abstract

The invention discloses preparation of a high-activity graphene-load platinum catalyst and application of the catalyst to a hydrogenation reaction of an aromatic nitro-compound, in particular to a high-activity catalyst used in a hydrogenation reaction of an aromatic nitro-compound and a preparation method thereof. A carrier of the catalyst is graphene; and an active ingredient is metal platinum.Specific to the current situation of small application range of graphene and large difficulty in large-scale preparation and application, ethylene glycol is taken as a reducing agent in the method, and Pt nanoparticles are successfully and uniformly loaded on a graphene oxide nano-sheet and are applied to the hydrogenation reaction of the aromatic nitro-compound, so that the high-activity graphene-load platinum catalyst represents catalytic activity which is remarkably superior to that of a Pt catalyst loaded with a normal carbon carrier.

Description

technical field [0001] The invention relates to the preparation of a highly active graphene-supported platinum catalyst and its application in the hydrogenation reaction of aromatic nitro compounds. [0002] Background technique [0003] Activated carbon is a porous carrier with a high specific surface area. It is the earliest type of carbon material used in catalyst carriers. It is often used to support noble metal active components, such as Pd, Pt, Ru, etc. On the basis of traditional activated carbon, people have developed new materials such as activated carbon felt and activated carbon cloth. Compared with conventional activated carbon, activated carbon felt and activated carbon cloth have faster adsorption-desorption rate, larger specific surface area, more uniform pore size distribution, faster equilibrium rate, and stronger liquid permeability. Although activated carbon has a large specific surface area, due to the large mass transfer resistance, it is difficult for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42C07C209/36C07C211/47C07C211/52C07C211/51C07C213/02C07C215/76
Inventor 侯昭胤聂仁峰王军华陈平秦玉
Owner ZHEJIANG UNIV
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