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Catalyst for preparing 1-aminoanthraquinone by hydrogenation of 1-nitroanthraquinone and its preparation method and application

A technology of nitroanthraquinone and catalyst, which is applied in the field of 1-nitroanthraquinone hydrogenation to prepare 1-aminoanthraquinone and its preparation field, which can solve the problems of poor catalyst selectivity, high cost, and easy deactivation, and achieve Effects of reduced catalyst consumption, increased yield, and easy recovery

Active Publication Date: 2019-06-04
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the disadvantages of poor selectivity, easy deactivation and high cost of related catalysts in the prior art, and provides a catalyst for preparing 1-aminoanthraquinone by hydrogenation of 1-nitroanthraquinone. The catalyst includes a carrier and an active component , the carrier is mesoporous carbon pretreated with ethylenediamine, the active components are palladium and silver,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a stirred autoclave, add 10%Pd-1%Ag / mesoporous carbon catalyst (the mesoporous carbon is treated with a 5wt% aqueous solution of ethylenediamine in advance; the percentages of Pd and Ag are their respective proportions of the catalyst The percentage of the total mass, the same below) 0.01g, 1-nitroanthraquinone 2.0g, distilled water 10ml, ammonium metavanadate 0.01g, close the reactor, replace the air in the reactor with nitrogen for three times, then replace the reactor with hydrogen Nitrogen in the medium for three times, and then filled with hydrogen to make the reaction pressure of the reactor reach 0.5MPa, heat the reactor to make the reaction temperature reach 120°C, start stirring, keep the constant temperature reaction until the pressure no longer drops, take out the reaction product, filter to remove the catalyst, Adopt liquid chromatography analysis, analysis result is listed in Table 1 (selectivity refers to the percentage that target product 1-aminoanthraq...

Embodiment 2

[0029] In a stirred autoclave, add 0.08 g of 8% Pd-1% Ag / mesoporous carbon catalyst (the mesoporous carbon is previously treated with an aqueous solution of ethylenediamine with a mass concentration of 1 wt%), 1-nitroanthraquinone 2.0 g, methanol 40ml, ammonium metavanadate 0.08g, close the reactor, replace the air in the reactor with nitrogen for three times, then replace the nitrogen in the reactor with hydrogen for three times, and then recharge hydrogen to make the reaction pressure of the reactor reach 1.0 MPa, heat the reactor to make the reaction temperature reach 100°C, start stirring, keep the temperature until the pressure no longer drops, take out the reaction product, remove the catalyst by filtration, and analyze by liquid chromatography, the analysis results are listed in Table 1.

Embodiment 3

[0031] In a stirred autoclave, add 0.02 g of 5% Pd-3% Ag / mesoporous carbon catalyst (the mesoporous carbon is previously treated with an aqueous solution of ethylenediamine with a mass concentration of 10 wt%), 1-nitroanthraquinone 2.0 g, isopropanol 40ml, ammonium metavanadate 0.02g, close the reactor, replace the air in the reactor with nitrogen for three times, then replace the nitrogen in the reactor with hydrogen for three times, and then charge hydrogen to make the reaction pressure of the reactor When it reaches 2.0MPa, heat the reaction kettle to make the reaction temperature reach 100°C, start stirring, keep the temperature until the pressure no longer drops, take out the reaction product, remove the catalyst by filtration, and analyze by liquid chromatography. The analysis results are listed in Table 1.

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PUM

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Abstract

The invention belongs to the technology of catalysts in the field of fine chemical engineering, and particularly relates to a catalyst used for preparing 1-amino-anthraquinone from 1-nitroanthraquinone by hydrogenation and a preparation method and application of the catalyst. Mesoporous carbon is added into ethylenediamine aqueous solution to be dipped, then, saline solution containing palladium and silver is used for dipping a carrier which is mesoporous carbon, and reduction, washing and filtering are carried out to obtain a Pd-Ag / mesoporous carbon catalyst. The above hydrogenation catalyst is used for preparing the 1-amino-anthraquinone from the 1-nitroanthraquinone by hydrogenation, a reaction condition is moderate, and product selectivity is high.

Description

technical field [0001] The invention belongs to catalyst technology in the field of fine chemical industry, and in particular relates to a catalyst for preparing 1-aminoanthraquinone by hydrogenation of 1-nitroanthraquinone, a preparation method and application thereof. Background technique [0002] Anthraquinone dyes are the second largest category of dyes after azo dyes, among which 1-aminoanthraquinone is an important intermediate for the synthesis of anthraquinone series dyes. It has the widest application and the largest consumption. The main raw material of azole anthraquinone. The market demand for 1-aminoanthraquinone continues to increase, especially the output of high-quality 1-aminoanthraquinone is far from meeting the market demand. [0003] The traditional production techniques include sulfonated ammonium solution method and sulfurized alkali method. The post-treatment of sulfonated ammonium solution will discharge mercury wastewater, which seriously damages t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/50B01J23/44C07C221/00C07C225/34
CPCB01J23/44B01J23/50C07C221/00C07C225/34
Inventor 陈政张伟鲁墨弘李明时
Owner CHANGZHOU UNIV
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