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Preparation method of catalyst for synthesis of aniline through catalytic hydrogenation of nitrobenzene

A catalytic hydrogenation and catalyst technology, which is applied in the preparation of amino compounds, the preparation of organic compounds, and metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of high cost of catalyst raw materials, complex catalyst preparation process, and poor catalyst stability. and other problems, to achieve the effect of simple operation, high selectivity and high conversion rate

Active Publication Date: 2013-09-04
GUANGXI UNIV
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the production of aniline by catalytic hydrogenation of nitrobenzene as a raw material has been applied industrially, there are still technical problems in the prior art such as complex catalyst preparation process, high cost of catalyst raw materials, and poor catalyst stability.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Preparation of Ni / bentonite catalyst: Take 5.0g of sodium bentonite and put it into a 1L beaker to make a suspension of 0.02g / L, then weigh nickel nitrate according to the ratio of Ni loading to 0.001mol / g bentonite and make it into a 0.2mol / L solution. Stir the sodium-based bentonite suspension and nickel nitrate solution in a water bath at 50°C at a constant temperature, and slowly drop in 0.4mol / L ammonia solution at a stirring speed of 250r / min until the pH of the solution is 9, age at room temperature for 24 hours and then depressurize After filtering, the filter cake was dried at 80°C for 10h and crushed to 200-300 meshes, and calcined at 250°C for 2h to obtain a Ni / bentonite catalyst with a Ni loading of 0.001mol / g bentonite. Using the catalyst to synthesize aniline by catalytic hydrogenation of nitrobenzene, the conversion rate of nitrobenzene is 78.45%, the yield of aniline is 75.12%, and the catalyst has a long cycle life.

Embodiment 2

[0018] Preparation of Ni / bentonite catalyst: Take 5.0g of sodium bentonite and put it into a 1L beaker to make a suspension of 0.02g / L, then weigh nickel nitrate according to the ratio of Ni loading to 0.002mol / g bentonite and make it into a 0.2mol / L solution. Stir the sodium-based bentonite suspension and nickel nitrate solution in a 70°C water bath at a constant temperature, and slowly drop in 0.4mol / L ammonia solution at a stirring speed of 250r / min until the pH of the solution is 9, age at room temperature for 24h and then depressurize After filtering, the filter cake was dried at 80°C for 10h and crushed to 200-300 meshes, and calcined at 300°C for 2h to obtain a Ni / bentonite catalyst with a Ni loading of 0.002mol / g bentonite. Using the catalyst to synthesize aniline by catalytic hydrogenation of nitrobenzene, the conversion rate of nitrobenzene is 85.60%, the yield of aniline is 74.95%, and the catalyst has a long cycle life.

Embodiment 3

[0020] Preparation of Ni / bentonite catalyst: Take 5.0g of sodium bentonite and put it into a 1L beaker to make a suspension of 0.02g / L, then weigh nickel nitrate according to the ratio of Ni loading to 0.003mol / g bentonite and make it into a 0.2mol / L solution. Stir the sodium-based bentonite suspension and nickel nitrate solution in a 70°C water bath at a constant temperature, and slowly drop in 0.4mol / L ammonia solution at a stirring speed of 250r / min until the pH of the solution is 9, age at room temperature for 24h and then depressurize After filtering, the filter cake was dried at 80°C for 10h and crushed to 200-300 meshes, and calcined at 300°C for 2h to obtain a Ni / bentonite catalyst with a Ni loading of 0.003mol / g bentonite. Using the catalyst to synthesize aniline by catalytic hydrogenation of nitrobenzene, the conversion rate of nitrobenzene is 99.96%, the yield of aniline is 81.88%, and the catalyst has a long cycle life.

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Abstract

The invention discloses a preparation method of a catalyst for synthesis of aniline through catalytic hydrogenation of nitrobenzene. The catalyst is obtained through loading nickel into bentonite. The catalyst is prepared by taking the sodium bentonite as the raw material and is prepared into a suspension liquid, the nickel nitrate solution is added into the suspension liquid, the sodium hydroxide or ammonium hydroxide or sodium carbonate is taken as the precipitator to enable the nickel to form hydroxide and load the hydroxide on the bentonite. The suspension liquid and the precipitate are filtered, dried at the temperature of 80 DEG C for 10 hours, and roasted at the temperature of 250 DEG C to 450 DEG C for 2 hours, to obtain the Ni-loaded bentonite catalyst with the content of Ni being 0.001-0.010mol / g in the bentonite. After being reduced through a reducing agent, the catalyst shows excellent activity in the synthesis of aniline through catalytic hydrogenation of nitrobenzene in a fixed bed reactor, and the recycling service life of the catalyst is relatively long.

Description

technical field [0001] The invention belongs to the field of heterogeneous catalysis. Specifically, it relates to a method for preparing a catalyst for synthesizing aniline by catalytic hydrogenation of nitrobenzene. Background technique [0002] Aniline is an important organic raw material, widely used in polyurethane, rubber additives, dyes and pigments, medicine and pesticides and other fields. Most of the rubber additives are based on aniline, such as rubber antioxidant RD and the important intermediate p-aminodiphenylamine of rubber antioxidant, which are synthesized from aniline. In addition, aniline is also an important raw material for the production of polyurethane raw material diphenylmethane diisocyanate (MDI), so aniline has great market development potential. At present, the catalytic hydrogenation of nitrobenzene is mainly used to produce aniline. The core of this process is an efficient catalyst. Therefore, it is of great theoretical value and practical sign...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755C07C211/46C07C209/36
Inventor 秦祖赠蒋月秀苏通明
Owner GUANGXI UNIV
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