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A kind of technique for synthesizing p-aminophenol by hydrogenation of nitrobenzene

A technology for p-aminophenol and nitrobenzene, which is applied in the field of catalytic reaction, can solve problems such as loss and need to be filtered and separated, and achieve the effects of stable reuse performance and simple equipment and process.

Active Publication Date: 2016-06-08
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to provide a simple method of immobilizing active groups on the surface of reactor components in view of the need for filtration, separation and loss of supported catalysts used in the synthesis of p-aminophenol in the current industrial production. Separately prepare active reaction components, and use active reaction components to carry out the method of nitrobenzene hydrogenation to synthesize p-aminophenol

Method used

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  • A kind of technique for synthesizing p-aminophenol by hydrogenation of nitrobenzene

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Effect test

Embodiment 1

[0023] In the first step, put 1.0g of Pt / C catalyst with 0.1% Pt load and 100g of solvent water into a 200ml tank reactor whose wall material is glass after being calcined at 100°C. A zirconium stirring blade and a thermocouple sleeve, the ratio of the surface area of ​​the metal member in contact with the reaction solution to the volume of the reaction solution is 0.1cm 2 / 1cm 3 ;

[0024] In the second step, in the above reactor, with N 2 After replacing the air for 8 to 12 minutes, pass H at a temperature of 80oC 2 , to H 2 The partial pressure is 0.1MPa, and the treatment time is 1 hour;

[0025] In the third step, after the treatment in the second step is completed, the reactor is lowered to room temperature, the catalyst is filtered, and the filtered catalyst can be used for related catalytic reactions after drying, and the filtrate can be reused as a treatment liquid for the next treatment process;

[0026] In the fourth step, the filtrate obtained by filtering in ...

Embodiment 2

[0031] In the first step, 0.4 g of Pt / Al with a Pt loading of 0.1% after calcination at 600 °C 2 0 3 Catalyst, 5g acetic acid, and 100g solvent water are put into a zirconium material tank reactor. The reactor is equipped with a stirring paddle, a thermocouple sleeve and a metal coil of the same material. The ratio of the surface area to the volume of the reaction solution is 2 cm 2 / 1cm 3

[0032] In the second step, in the above reactor, with N 2 After replacing the air for 8 to 12 minutes, pass H at a temperature of 180oC 2 , to H 2 The partial pressure is 0.5MPa, and the treatment time is 10 hours;

[0033] In the third step, after the treatment in the second step is completed, the reactor is lowered to room temperature, the catalyst is filtered, and the filtered catalyst can be used for related catalytic reactions after drying, and the filtrate can be reused as a treatment liquid for the next treatment process;

[0034] In the fourth step, the filtrate obtained by fi...

Embodiment 3

[0039] In the first step, 5 g of Pt / Al with a Pt loading of 0.01% after calcination at 300 °C 2 0 3 Catalyst, 0.1g citric acid, and 100g solvent water are put into a zirconium material tank reactor. The reactor is equipped with a stirring paddle, a thermocouple sleeve and a metal coil of the same material. The metal components and the reaction The ratio of the surface area in contact with the liquid to the volume of the reaction liquid is 5 cm 2 / 1cm 3 ;

[0040] In the second step, in the above reactor, with N 2 After replacing the air for 8-12 minutes, pass H at a temperature of 120oC 2 , to H 2 The partial pressure is 0.2MPa, and the treatment time is 4 hours;

[0041] In the third step, after the treatment in the second step is completed, the reactor is lowered to room temperature, the catalyst is filtered, and the filtered catalyst can be used for related catalytic reactions after drying, and the filtrate can be reused as a treatment liquid for the next treatment pr...

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Abstract

The present invention relates to a process for synthesizing p-aminophenol through nitrobenzene hydrogenation. The process comprises: adding water, concentrated sulfuric acid, zinc sulfate, nitrobenzene and a surfactant hexadecyl trimethyl ammonium bromide to a reactor provided with an active reaction member according to a mass ratio of concentrated sulfuric acid to zinc sulfate to nitrobenzene to hexadecyl trimethyl ammonium bromide to water of 0-20:0-2:2-20:0.01:100; and adopting N2 to replace air for 8-12 min, heating to a reaction temperature of 80-200 DEG C, introducing H2 to achieve a hydrogen partial pressure of 0.1-2.0 MPa, and carrying out a reaction for 3-8 h to make the nitrobenzene convert into the p-aminophenol. According to the present invention, the active reaction member is adopted to synthesize the p-aminophenol through nitrobenzene hydrogenation, wherein the highest p-aminophenol yield is 83.7%, the repeated use performance is stable, the reaction result does not significantly change after repeating the reaction more than 50 times, and the catalyst loss and regeneration problems are not produced during the reaction process.

Description

technical field [0001] The invention belongs to the field of catalytic reaction, and in particular relates to a method for preparing an active reaction component by immobilizing an active component on the surface of a reactor component, and then using the active reaction component to hydrogenate nitrobenzene to synthesize p-aminophenol. Background technique [0002] p-Aminophenol (p-Aminophenol, referred to as PAP) is a widely used intermediate in organic synthesis, widely used in dyes, medicine, rubber and other fields. In the pharmaceutical industry, p-aminophenol is an intermediate for the synthesis of acetaminophen, paramethacin, anoxamine, vitamin B1, and the complex agent nicotinamide; in the rubber industry, p-aminophenol is mainly used for anti-aging agents 4010MA, 4020, 4030, etc. The synthesis of these products is the matching anti-aging agent for the promising radial tire products. At present, the production of p-aminophenol is divided into p-nitrophenol method a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/76C07C213/00
CPCY02P20/584
Inventor 王淑芳王玲张东升王延吉赵新强
Owner HEBEI UNIV OF TECH
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