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High-selectivity reduction catalyst for nitro-aromatic hydrocarbon as well as preparation method and application of high-selectivity reduction catalyst

A nitroaromatic, high-selectivity technology, applied in the preparation of amino compounds, preparation of amino hydroxyl compounds, chemical instruments and methods, etc., to achieve the effects of good stability, broad industrial application prospects and low carbonization temperature

Pending Publication Date: 2021-11-19
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, using hydrogen as a reducing agent, there is still no platinum group metal catalyst that can achieve 100% conversion of aromatic nitro compounds at room temperature and obtain 100% product selectivity at the same time.

Method used

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  • High-selectivity reduction catalyst for nitro-aromatic hydrocarbon as well as preparation method and application of high-selectivity reduction catalyst
  • High-selectivity reduction catalyst for nitro-aromatic hydrocarbon as well as preparation method and application of high-selectivity reduction catalyst
  • High-selectivity reduction catalyst for nitro-aromatic hydrocarbon as well as preparation method and application of high-selectivity reduction catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] A kind of synthetic method of nitroaromatics highly selective reduction catalyst of the present embodiment, comprises the steps:

[0047] (1) Preparation of Ir@H102 complex: weigh 210mg NaHCO 3 and 1180mg H102 in a 50mL three-neck round bottom flask, add 15mL isopropanol, stir for 30min until the hyperbranched product is completely dissolved; then add 5mL 0.1mol L -1 IrCl 3 isopropanol solution, stirred for 30 minutes to make the solution evenly mixed; the mixed solution was ultrasonically treated for 10 minutes, and then passed into N 2 Remove the air; finally, put the reaction bottle into the oil bath and keep it open to N 2 state, react at a constant temperature of 100°C for 60 minutes; stop the reaction, and cool to room temperature. The isopropanol was removed by rotary evaporation at 45°C to obtain the Ir@H102 complex.

[0048] (2) Preparation of Ir@H102-350 catalyst: Transfer the Ir@H102 composite to a porcelain boat, place it in a constant temperature blast ...

Embodiment 2

[0056] A kind of synthetic method of nitroaromatics highly selective reduction catalyst of the present embodiment, comprises the steps:

[0057] (1) Preparation of Ir@H102 complex: weigh 210mg NaHCO 3 and 1180mg H102 in a 50mL three-neck round bottom flask, add 15mL isopropanol, stir for 30min until the hyperbranched product is completely dissolved; then add 5mL 0.1mol L -1 IrCl 3 isopropanol solution, stirred for 30 minutes to make the solution evenly mixed; the mixed solution was ultrasonically treated for 10 minutes, and then passed into N 2 Remove the air; finally, put the reaction bottle into the oil bath and keep it open to N 2 state, react at a constant temperature of 100°C for 60 minutes; stop the reaction, and cool to room temperature. The isopropanol was removed by rotary evaporation at 45°C to obtain the Ir@H102 complex.

[0058] (2) Preparation of Ir@H102-400 catalyst: Transfer the Ir@H102 composite to a porcelain boat, place it in a constant temperature blast ...

Embodiment 3

[0061] A kind of synthetic method of nitroaromatics highly selective reduction catalyst of the present embodiment, comprises the steps:

[0062] (1) Preparation of Ir@H102 complex: weigh 210mg NaHCO 3 and 1180mg H102 in a 50mL three-neck round bottom flask, add 15mL isopropanol, stir for 30min until the hyperbranched product is completely dissolved; then add 5mL 0.1mol L -1 IrCl 3 isopropanol solution, stirred for 30 minutes to make the solution evenly mixed; the mixed solution was ultrasonically treated for 10 minutes, and then passed into N 2 Remove the air; finally, put the reaction bottle into the oil bath and keep it open to N 2 state, react at a constant temperature of 100°C for 60 minutes; stop the reaction, and cool to room temperature. The isopropanol was removed by centrifugation at room temperature to obtain the Ir@H102 complex.

[0063] (2) Preparation of Ir@H102-350C catalyst: Transfer the Ir@H102 composite to a porcelain boat, place it in a constant temperatu...

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Abstract

The invention belongs to the technical field of nano materials and preparation thereof, and particularly discloses a high-selectivity reduction catalyst for nitro-aromatic hydrocarbon as well as a preparation method and application of the high-selectivity reduction catalyst. Iridium trichloride is used as a metal precursor, isopropanol / ethanol is used as a solvent and a reducing agent, a hydroxyl-terminated hyperbranched polymer (H102) is used as a carrier, supramolecular self-assembly of H102 in isopropanol / ethanol is utilized, a N2 introduction state is kept, an oil bath reaction is performed for 1 h at the temperature of 100 DEG C, and an Ir@H102 compound is prepared; and the Ir@H102 is calcined in an inert atmosphere at the temperature of 350-400 DEG C (T) for 2 hours to prepare the novel composite nano material Ir@H102-T supported by a hyperbranched carbon skeleton. The Ir@H102-350 is applied to catalytic hydrogenation of nitro-aromatic hydrocarbon, nitrobenzene and derivatives thereof can be subjected to rapid and high-selectivity hydro-conversion into corresponding arylamine at room temperature, hydrogenation reaction is performed for 30 min at room temperature (25 DEG C) and under H2 pressure of 1.5 MPa, 100% conversion of nitro-aromatic hydrocarbon and 99.9% selectivity of corresponding arylamine can be achieved, and the catalyst is extremely good in stability and reusability and wide in industrial application prospect.

Description

technical field [0001] The invention relates to the technical field of novel nanomaterials and their preparation, in particular to a highly selective reduction catalyst for nitroaromatics and its preparation method and application. Background technique [0002] Aromatic amine compounds are important organic chemical raw materials and fine chemical intermediates, usually made from aromatic nitro compounds through deep processing, and are widely used in the production of pharmaceuticals, rubber, dyes, pesticides and other fine chemicals It occupies a very important position in chemical production. People have been trying to realize the rapid and efficient conversion of aromatic nitro compounds at room temperature. However, until now, the selective synthesis of aromatic amines from aromatic nitro compounds still requires a long reaction time or a high reaction temperature or a large hydrogen pressure. How to achieve 100% conversion rate and 100% selectivity of aromatic amines...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J35/08B01J35/02C07C209/36C07C211/45C07C211/52C07C213/02C07C215/68C07C225/22
CPCB01J23/468C07C209/36C07C213/02C07C215/68B01J35/50B01J35/51C07C211/45C07C211/52C07C225/22
Inventor 黄涛张明明赵燕熹张道洪
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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