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Catalyzer for synthesizing p-aminophenol by nitrobenzene catalytic hydrogenation as well as method for preparing and applying the same

A technology for catalytic hydrogenation of p-aminophenol, which is applied in the preparation of organic compounds, preparation of aminohydroxyl compounds, organic compound/hydride/coordination complex catalysts, etc., can solve environmental pollution of wastewater discharge, harsh reaction conditions, equipment Corrosion and other problems, to achieve the effect of good stability, high mechanical strength and low cost

Inactive Publication Date: 2008-05-14
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by the present invention is to provide a catalyst for synthesizing p-aminophenol by catalytic hydrogenation of nitrobenzene and its preparation and application method. The catalyst is a highly active heterogeneous catalyst, which overcomes the existing It has the disadvantage that homogeneous catalysts cannot be reused, and overcomes the disadvantages of harsh reaction conditions and low activity of existing heterogeneous catalysts, and also overcomes the problems of equipment corrosion and wastewater discharge environmental pollution

Method used

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  • Catalyzer for synthesizing p-aminophenol by nitrobenzene catalytic hydrogenation as well as method for preparing and applying the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Synthesis of room temperature ionic liquid N,N,N-trimethyl-N-sulfobutyl-ammonium bisulfate:

[0044] In the first step, take an aqueous solution of trimethylamine containing 0.50 mol of trimethylamine and 0.55 mol of 1,4-butane sultone, put them in a 250ml three-necked flask, and react at room temperature to 60°C for 8 to 48 hours. After the reaction solution was taken out, water was distilled off under reduced pressure to obtain a white zwitterionic solid, which was washed sequentially with absolute ethanol, toluene and anhydrous ether, and then vacuum-dried at 80°C to constant weight to obtain amphoteric Ion N,N,N-trimethyl-N-sulfobutylammonium, the weight content of trimethylamine in the trimethylamine aqueous solution is more than or equal to 33%.

[0045] In the second step, take 0.50mol of the zwitterion N,N,N-trimethyl-N-sulfobutylammonium prepared in the first step and put it into a four-necked flask, and slowly drop the Add 0.48-0.52 mol of concentrated sulfur...

Embodiment 2

[0048] In the first step, weigh 10ml (9.356g) of tetraethyl orthosilicate and place it in a reactor, add 2ml of absolute ethanol and 30ml of deionized water, and stir evenly in a 90°C water bath;

[0049] In the second step, take by weighing the room temperature ionic liquid N, N, N-trimethyl-N-sulfobutyl-ammonium bisulfate 0.142g and chloroplatinic acid 0.754mg (equivalent to metal platinum is 0.284mg ), which is added to the reactor of the first step, stirred until a gel is formed, and then aged at room temperature for 24 hours;

[0050] In the third step, the material obtained in the second step is vacuum-dried at 100° C. for 0.5 hours;

[0051] In the fourth step, the dried substance in the third step is roasted in a muffle furnace at 120° C. for 5 hours in a nitrogen atmosphere or an air atmosphere;

[0052] In the fifth step, the material obtained in the fourth step is placed in a tubular reactor, and the volume ratio is N 2 :H 2 = 2:1 N 2 and H 2 The mixed gas was ...

Embodiment 3

[0055] In the first step, weigh 10ml (9.356g) of ethyl orthosilicate and place it in a reactor, add 40ml of absolute ethanol and 4ml of deionized water, and stir evenly in a water bath at 30°C;

[0056] In the second step, take by weighing the room temperature ionic liquid N, N, N-trimethyl-N-sulfobutyl-ammonium bisulfate 2.7g and chloroplatinic acid 0.215g (equivalent to metal platinum is 0.081g ), adding it into the reactor of the first step, stirring until a gel is formed, and aging at 100° C. for 10 hours;

[0057] In the third step, the material obtained in the second step is vacuum-dried at 30° C. for 24 hours;

[0058] In the fourth step, the dried substance in the third step is roasted in a muffle furnace at 250° C. for 1 hour in a nitrogen atmosphere or an air atmosphere;

[0059] In the fifth step, the material obtained in the fourth step is placed in a tubular reactor, and the volume ratio is N 2 :H 2 = 2:1 N 2 and H 2 The mixed gas is used as reducing gas, red...

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Abstract

The invention relates to a catalyst used for synthesis of p-aminophenol by catalytic hydrogenation of nitrobenzene, a preparation method and an application method, belonging to catalyst containing both platinum and organic compound field. The catalyst is a supported and bi-functional catalyst, and comprises room temperature ionic liquid of N, N, N-trimethyl-N-sulfobutyl-ammonium bisulfate which is one component of the active components, active metal Pt which is the other component of the active components, and silica gel carrier; wherein, the loading of the room temperature ionic liquid of N, N, N-trimethyl-N-sulfobutyl-ammonium bisulfate is 5 to 50%, while the loading of the active metal Pt is 0.01 to 1.5%. The invention has the advantages that: as a highly active heterogeneous catalyst, the catalyst overcomes the shortcomings that the homogeneous catalyst in prior art can not be used repeatedly, the reaction conditions of the heterogeneous catalyst in prior art are severe and the activity is low, and the problems that the equipment is liable to corrosion and the discharge of wastewater pollutes environment are solved.

Description

technical field [0001] The technical scheme of the present invention relates to a catalyst containing platinum and an organic compound, in particular to a catalyst for synthesizing p-aminophenol by catalytic hydrogenation of nitrobenzene and its preparation and application method. technical background [0002] The method for synthesizing p-aminophenol by catalytic hydrogenation of nitrobenzene is generally considered to be the future development direction of synthesizing p-aminophenol. The catalytic hydrogenation technology of nitrobenzene has the advantages of one-step reaction, simple method, less steps, relatively mild equipment and process conditions, etc., and is suitable for large-scale industrial production of p-aminophenol. [0003] The mechanism of nitrobenzene catalytic hydrogenation synthesis p-aminophenol reaction is: [0004] [0005] The first step of the reaction, that is, the catalytic hydrogenation of nitrobenzene to generate phenylhydroxylamine, uses a ...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J23/42C07C215/76C07C213/00
Inventor 王延吉崔咏梅赵新强
Owner HEBEI UNIV OF TECH
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