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Method for preparing catalyst for nitro reduction and application

A catalyst and nitro technology, applied in the field of preparing catalysts for nitro reduction, can solve the problems of insufficient catalyst performance, low catalyst use efficiency, insufficient stability and activity, etc., to promote hydrogen dissociation and overflow, The effect of enhancing stability and activity and reducing production cost

Active Publication Date: 2020-01-17
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many kinds of palladium carbon catalysts on the market, and some catalysts have been used in general use. In the nitro reduction reaction system, due to the lack of stability and activity of palladium carbon catalysts, the catalyst life decays significantly. In addition, due to the reaction type, Due to the influence of physical and chemical parameters and reaction conditions, the performance of the catalyst cannot be fully exerted, and the use efficiency of the catalyst is usually not high. Therefore, it is particularly important to design and prepare a highly active palladium carbon catalyst for the nitro reduction reaction.

Method used

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  • Method for preparing catalyst for nitro reduction and application
  • Method for preparing catalyst for nitro reduction and application
  • Method for preparing catalyst for nitro reduction and application

Examples

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Effect test

Embodiment 1

[0029] The method for preparing the catalyst for nitro reduction in this embodiment comprises the following steps:

[0030] Step 1. Place 100 g of activated carbon in 1000 g of hydrochloric acid solution with a mass concentration of 5%, carry out cooking treatment at 110° C. for 0.5 h, filter, wash the retentate with pure water until the pH is 6, and obtain acid-treated activated carbon;

[0031] Step 2, place the acid-treated activated carbon described in step 1 in 600 g of potassium hydroxide solution with a mass concentration of 15%, carry out cooking treatment at 80° C. for 0.5 h, filter, and wash the retentate with pure water until the pH is 8 , to obtain alkali-treated activated carbon;

[0032] Step 3, place the alkali-treated activated carbon described in step 2 in 1500 g of hydrogen peroxide with a mass concentration of 10%, carry out cooking treatment at 100° C. for 4 hours, filter, wash the retentate with pure water until the pH is 6, filter, and obtain the oxidized...

Embodiment 2

[0037] The method for preparing the catalyst for nitro reduction in this embodiment comprises the following steps:

[0038] Step 1. Place 100 g of activated carbon in 800 g of 5% hydrochloric acid solution, cook at 100° C. for 0.5 h, filter, wash the retentate with pure water until the pH is 6, and obtain acid-treated activated carbon;

[0039] Step 2, place the acid-treated activated carbon described in step 1 in 600 g of potassium hydroxide solution with a mass concentration of 20%, carry out cooking treatment at 80° C. for 1 h, filter, and wash the retentate with pure water until the pH is 8. Obtain alkali-treated activated carbon;

[0040] Step 3, place the alkali-treated activated carbon described in step 2 in 1500 g of hydrogen peroxide with a mass concentration of 10%, carry out cooking treatment at 100° C. for 3 h, filter, wash the retentate with pure water until the pH is 6, filter, and obtain the oxidized Activated carbon, the oxidized activated carbon is mixed with w...

Embodiment 3

[0049] The method for preparing the catalyst for nitro reduction in this embodiment comprises the following steps:

[0050] Step 1. Place 100 g of activated carbon in 600 g of hydrochloric acid solution with a mass concentration of 2%, carry out cooking treatment at 80° C. for 1 hour, filter, wash the retentate with pure water until the pH is 6, and obtain acid-treated activated carbon;

[0051] Step 2, place the acid-treated activated carbon described in step 1 in 500 g of a sodium hydroxide solution with a mass concentration of 15%, carry out cooking treatment at 70° C. for 2 h, filter, and wash the retentate with pure water until the pH is 8. Obtain alkali-treated activated carbon;

[0052] Step 3, place the alkali-treated activated carbon described in step 2 in 1000 g of nitric acid solution with a mass concentration of 5%, carry out cooking treatment at 110° C. for 2 h, filter, wash the retentate with pure water until the pH is 6, filter, and obtain the oxidized After ac...

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Abstract

The invention discloses a method for preparing a catalyst for nitro reduction. The method comprises the steps: (1) cooking activated charcoal in hydrochloric acid; (2) cooking the acid treated activated charcoal in an alkaline solution; (3) cooking the alkali treated activated charcoal in an oxidant solution, and carrying out pulping; (4) mixing a palladium chloride solution, a dispersant and oxidated activated charcoal pulp, carrying out stirring, and carrying out aging, so as to obtain a suspension; or mixing assistant metal with the oxidated activated charcoal pulp, carrying out stirring and pulping, then, mixing the palladium chloride solution, the dispersant and the assistant loaded activated charcoal pulp, carrying out stirring, and carrying out aging, so as to obtain the suspension;and (5) subjecting the suspension to reduction, thereby obtaining the catalyst for nitro reduction. In addition, the invention further provides an application of the catalyst prepared by adopting theabove-mentioned method in a hydrogenation reaction of o-nitroaniline. In a nitro reduction reaction of the o-nitroaniline, the catalyst shows superior performance, the pressure drop is 0.28MPa or more, and the yield is 85.2% or more.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a method and application for preparing a catalyst for nitro group reduction. Background technique [0002] Palladium carbon catalyst is a new type of material prepared by loading the precious metal palladium on the carrier activated carbon. It has the characteristics of small feeding amount, high activity, stable performance, green environmental protection and easy recycling. It is widely used in the pharmaceutical industry, petrochemical industry, Dye fragrance industry, electronics industry and other fine chemical hydrogenation reduction process. In the synthesis of fine chemicals, palladium-carbon catalysts are mainly used in hydrogenation and oxidation reactions: triple bond hydrogenation, double bond hydrogenation, carbonyl hydrogenation, nitro reduction and hydroxyl oxidation, phenolic hydroxyl oxidation, etc. As an irreplaceable auxiliary material...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J23/44C07C209/36C07C211/51
CPCB01J23/8913B01J23/44C07C209/36C07C211/51Y02P20/584
Inventor 翟康张涵王昭文张磊程杰张力李岳锋万克柔
Owner XIAN CATALYST NEW MATERIALS CO LTD
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