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Hydrogenation catalyst and preparation method and application thereof

A technology of hydrogenation catalysts and oxides, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve the problems of poor selectivity of azobenzene compounds

Active Publication Date: 2020-04-21
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the selectivity of azobenzene compounds is very poor, and the generated azobenzene compounds are easily overhydrogenated to form azobenzene compounds and aniline
Therefore, the selective preparation of azobenzene oxides by hydrogenation of nitroaromatics remains a great challenge.

Method used

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  • Hydrogenation catalyst and preparation method and application thereof
  • Hydrogenation catalyst and preparation method and application thereof
  • Hydrogenation catalyst and preparation method and application thereof

Examples

Experimental program
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preparation example Construction

[0031] The present invention provides the preparation method of hydrogenation catalyst described in above-mentioned technical scheme, comprises the following steps:

[0032] A supported gold nanomaterial is provided, the supported gold nanomaterial includes a carrier and gold nanoparticles loaded on the carrier;

[0033] coating the suspension containing the supported gold nanomaterial on the surface of the substrate, and forming a supported gold nanomaterial layer on the surface of the substrate after drying;

[0034] The atomic layer deposition method is used to deposit the gold nano particles on the surface of the supported gold nano material layer to form metal oxides in the form of single atom dispersion, and the hydrogenation catalyst is obtained after removing the substrate.

[0035]The present invention firstly provides a supported gold nanomaterial, which includes a carrier and gold nanoparticles loaded on the carrier. In the present invention, there is no special li...

Embodiment 1

[0051] (1) First prepare gold nanomaterials supported by titanium oxide by impregnation-reduction method (reference: Reduction of Nitroaromatic Compounds on Supported Gold Nanoparticles by Visible and Ultraviolet Light, Angew.Chem.2010, 122, 9851-9855), denoted as Au / TiO 2 , where the Au content is 3.0wt.%, and then the Au / TiO 2 Mix with ethanol, disperse evenly to obtain a suspension, in which Au / TiO 2 The concentration is 0.01g / mL, the suspension is coated on the surface of a glass sheet (8cm×8cm in size), and Au / TiO2 is formed on the surface of the glass sheet after natural drying at room temperature 2 layer (thickness≤0.15cm);

[0052] (2) will contain Au / TiO 2 The glass sheet of the first layer is placed in the atomic layer deposition chamber (the volume of the atomic layer deposition chamber is about 500cm 3 ), the Au / TiO 2 Nickel oxide in the form of monatomic dispersion was deposited on the surface of the layer. The deposition parameters were set as follows: the ...

Embodiment 2

[0065] The method for preparing hydrogenation catalyst with reference to embodiment 1, differs from embodiment 1 in that, Au / TiO 2 The metal oxide deposited on the surface in the form of monatomic dispersion is iron oxide; specifically, the deposition parameters set in this embodiment are: the reaction temperature is 280°C, the temperature of the reaction source ferrocene is 70°C, and the ozone The temperature is 30°C, and the nitrogen flow rate is 50 sccm; specifically, the ferrocene vapor is first pulsed into the atomic layer deposition chamber, the pulse time is 7 seconds, the gas holding time is 10 seconds, and the purge time is 25 seconds, and then the ozone pulse is injected into the chamber. In the atomic layer deposition chamber, the pulse time is 1 second, the gas holding time is 10 seconds, and the purge time is 25 seconds. So far, one deposition process is completed; the deposition process is repeated for a total of 15 deposition processes, and the monoatomic dispers...

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Abstract

The invention provides a hydrogenation catalyst and a preparation method and application thereof, and belongs to the technical field of selective catalytic hydrogenation. The hydrogenation catalyst provided by the invention comprises a carrier and gold nanoparticles loaded on the carrier, wherein the surfaces of the gold nanoparticles are modified with metal oxides existing in a monoatomic dispersion form. According to the hydrogenation catalyst provided by the invention, the surfaces of the gold nanoparticles are modified on a monatomic scale by utilizing the metal oxide, an azoxybenzene compound is selectively generated when nitro-aromatic hydrocarbon hydrogenation is catalyzed, the reactant conversion rate is high, and the product selectivity is good. The result of the embodiment showsthat when the hydrogenation catalyst provided by the invention is used for catalyzing the hydrogenation reaction of nitro-aromatic hydrocarbon, the conversion rate of the reactant nitro-aromatic hydrocarbon is up to 100%, and the selectivity of the product azoxybenzene compound is up to 98.4%.

Description

technical field [0001] The invention relates to the technical field of selective catalytic hydrogenation, in particular to a hydrogenation catalyst and its preparation method and application. Background technique [0002] Azobenzene compounds are important intermediates in organic synthesis, widely used in the fields of chemical stabilizers, polymerization inhibitors, dyes and pigments, and can also be used as raw materials for the preparation of electronic display materials and medicines. At present, azobenzene oxide compounds are mainly prepared from nitroaromatics, and the common preparation methods mainly include zinc powder reduction method, formaldehyde reduction method, β-cyclodextrin reduction method, sodium borohydride reduction method, etc. Among them, the zinc powder reduction method is a more traditional method. The main problem of this method is that it consumes more zinc powder, and the zinc oxide produced is difficult to recycle; the formaldehyde reduction met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89C07C245/08
CPCB01J23/892C07C245/08B01J35/394
Inventor 覃勇陈朝秋赵吉晓杨杰张佰艳
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI