Hydrogenation reducing method for aromatic nitro-compound

A technology for aromatic nitro compounds, applied in the field of hydrogenation and reduction of aromatic nitro compounds, can solve the problems of difficult separation and recovery, unstable homogeneous catalysts, etc., and achieve good chemical stability, small particle size, and difficult aggregation Effect

Inactive Publication Date: 2006-08-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There have been some reports on the use of homogeneous catalysts to catalyze this reaction, however, these homogeneous catalysts are unstable in air and are not easily separated and recovered from the reactants

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] This example illustrates the preparation of spherical supports for catalysts used in the process of the invention.

[0026] 189g Na 2 SiO 3 9H 2 O was dissolved in 1000 mL of distilled water, and 3 mol / L HCl solution was slowly added dropwise under stirring condition to adjust the pH value of the solution to 13, and filtered for later use.

[0027] Add 42.2 g of FeCl to a 3 L stirred tank with 1200 mL of distilled water 3 ·6H 2 O and 20.6gFeCl 2 4H 2 O, heat up to 85-90°C, add 60mL of 25% NH during high-speed stirring 3 ·H 2 O solution, after stirring at high speed for 3 minutes, use a magnetic separator to separate Fe 3 o 4 Nanoparticle products. The washed precipitated product was ultrasonically dispersed in the above pretreated Na 2 SiO 3 solution, and then moved into a 3L stirred tank, heated to 85°C, under nitrogen protection and stirring conditions, slowly added HCl solution with a concentration of about 2mol / L to the solution, within about 3 hours, th...

Embodiment 2

[0034] This example illustrates the preparation of the palladium catalyst used in the process of the present invention.

[0035] Get the spherical carrier 10g that embodiment 1 prepares, PdCl 2 Add hydrochloric acid to prepare 30ml of impregnation solution with Pd content of 0.35wt% and pH4.5, impregnate the carrier for 2 hours at room temperature, and impregnate the PdCl 2 The carrier was dried in an oven at 70°C for 2 hours, at 120°C for 2 hours, then calcined in a muffle furnace at 300°C for 4 hours, and then reduced with hydrogen at 100°C for 4 hours. The prepared catalyst was designated as Catalyst-1. The Pd content in the catalyst was 1.0 wt%.

Embodiment 3

[0037] This example illustrates the preparation of the platinum catalyst used in the process of the invention.

[0038] Get the spherical carrier 10g that embodiment 1 prepares, H 2 PtCl 6 Add hydrochloric acid to make 30ml of impregnating solution with Pt content 0.35wt%, pH4.5, impregnate carrier at normal temperature for 2 hours, impregnate H 2 PtCl 6 The carrier was dried in an oven at 70°C for 2 hours, at 120°C for 2 hours, then calcined in a muffle furnace at 500°C for 4 hours, and then reduced with hydrogen at 400°C for 4 hours. The prepared catalyst was designated as Catalyst-2. The Pt content in the catalyst was 1.0 wt%.

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Abstract

The method of hydrogenising aromatic nitro compound is that inside slurry bed or fluidized bed, in the presence of magnetic noble catalyst and under the conditions of reaction temperature 25-150 deg.c, reaction pressure 0.1-3.0 MPa and hydrogen / liquid material volume ratio of 5-300, aromatic nitro compound and hydrogen are contact reacted. The magnetic noble catalyst consists of spherical carrier comprising alumina and magnetic grain and one or several of noble Pt, Pd, Ru and Rh as active component, and the magnetic grain consists of SiO2 coating layer and ferric material kernal. The catalyst with superparamagnetism may be separated and recovered easily from reaction product under the action of magnetic field.

Description

technical field [0001] The invention relates to a method for hydrogenation reduction of aromatic nitro compounds. More specifically, it relates to a method for hydrogenating and reducing aromatic nitro compounds with a magnetic noble metal catalyst in a slurry bed or a fluidized bed. Background technique [0002] Hydrogenation of aromatic nitro compounds is a very important unit reaction in dyestuff, medicine and fragrance industry. There have been some reports on the use of homogeneous catalysts to catalyze this reaction, however, these homogeneous catalysts are unstable in air and are not easy to separate and recover from the reactants. In recent years, the use of supported palladium, platinum, rhodium catalysts and Raney nickel catalysts for the hydrogenation of aromatic nitro compounds to aromatic amines has attracted people's attention. [0003] USP5,877,350 discloses a method for the hydrogenation of aromatic nitro compounds to prepare aromatic amines. The method is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/36
Inventor 孟祥堃卢立军张晓昕宗保宁慕旭宏闵恩泽
Owner CHINA PETROLEUM & CHEM CORP
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