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A kind of preparation method and application of catalyst for n-methylaniline synthesis

A technology of methylaniline and catalyst, which is applied in the field of chemical technology, can solve the problems of danger, inconvenience, inconvenient use, etc., and achieve the effect of avoiding hydrogenation reduction pretreatment and excellent catalytic performance

Active Publication Date: 2020-03-20
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, hydrogenation reduction pretreatment has certain risks and inconveniences, and is inconvenient to use to a certain extent.

Method used

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  • A kind of preparation method and application of catalyst for n-methylaniline synthesis

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Accurately measure 87.5mL (0.00875mol) of 0.1mol / L copper nitrate aqueous solution, 262.5mL (0.02625mol) of 0.1mol / L zinc nitrate aqueous solution, 175mL (0.0175mol) of 0.1mol / L chromium nitrate and 0.1 Mix 525 mL (0.0525 mol) of mol / L aluminum nitrate thoroughly, take 0.1 mol / L sodium hydroxide aqueous solution as a precipitant, and use the co-precipitation method to allow the nitrate mixed solution and sodium hydroxide aqueous solution to react in a 60°C water bath to pH After reaching 10, age for 10 hours;

[0019] (2) centrifuging the aged system in step (1), washing the obtained filter cake until the pH value is 7 and drying at 80° C. under normal pressure for 10 hours to obtain a copper-zinc-chromium-aluminum quaternary coprecipitate;

[0020] (3) placing the co-precipitate obtained in step (2) in a 900°C muffle furnace for roasting for 6h, and cooling naturally;

[0021] (4) Mix the mixture obtained in step (3) with alumina, pseudoboehmite, and 15wt% nitric ...

Embodiment 2

[0025] (1) Accurately measure 116.7mL (0.01167mol) of 0.1mol / L copper nitrate aqueous solution, 233.3mL (0.02333mol) of 0.1mol / L zinc nitrate aqueous solution, 175mL (0.0175mol) of 0.1mol / L chromium nitrate and 0.1 Mix 525 mL (0.0525 mol) of mol / L aluminum nitrate thoroughly, take 0.1 mol / L sodium hydroxide aqueous solution as a precipitant, and use the co-precipitation method to allow the nitrate mixed solution and sodium hydroxide aqueous solution to react in a 60°C water bath to pH After reaching 10, age for 10 hours;

[0026] (2) centrifuging the aged system in step (1), washing the obtained filter cake until the pH value is 7 and drying at 80° C. under normal pressure for 10 hours to obtain a copper-zinc-chromium-aluminum quaternary coprecipitate;

[0027] (3) placing the co-precipitate obtained in step (2) in a 900°C muffle furnace for roasting for 6h, and cooling naturally;

[0028] (4) Mix the mixture obtained in step (3) with alumina, pseudoboehmite, and 15wt% nitric...

Embodiment 3

[0032] (1) Accurately measure 175mL (0.0175mol) of 0.1mol / L copper nitrate aqueous solution, 175mL (0.0175mol) of 0.1mol / L zinc nitrate aqueous solution, 175mL (0.0175mol) of 0.1mol / L chromium nitrate and 0.1mol / L 525 mL (0.0525 mol) of aluminum nitrate in L was fully mixed, and 0.1 mol / L sodium hydroxide aqueous solution was used as a precipitating agent, and the nitrate mixed solution and sodium hydroxide aqueous solution were reacted in a water bath at 60°C until the pH reached 10 by co-precipitation method. Afterwards, aging for 10 hours;

[0033] (2) centrifuging the aged system in step (1), washing the obtained filter cake until the pH value is 7 and drying at 80° C. under normal pressure for 10 hours to obtain a copper-zinc-chromium-aluminum quaternary coprecipitate;

[0034] (3) placing the co-precipitate obtained in step (2) in a 900°C muffle furnace for roasting for 6h, and cooling naturally;

[0035] (4) Mix the mixture obtained in step (3) with alumina, pseudoboeh...

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Abstract

The invention belongs to the field of chemical processes, and in particular relates to a preparation method of a catalyst for synthesis of N-methylaniline and application. The catalyst is a copper-zinc-chromium-aluminum spinel catalyst, the catalyst does not need hydrogenation reduction pretreatment before being used, the single pass conversion rate of aniline is as high as 90% or more, and the selectivity of the N-methylaniline is as high as 98% or more.

Description

technical field [0001] The invention belongs to the field of chemical technology, and in particular relates to a preparation method and application of a catalyst used for the synthesis of N-methylaniline. Background technique [0002] N-Methylaniline has excellent anti-knock properties and is an important intermediate widely used in the fields of medicine, pesticides and dyes. The methods for synthesizing N-methylaniline are mainly divided into liquid phase synthesis and gas phase synthesis. The liquid-phase synthesis method is gradually replaced by the gas-phase synthesis method due to the use of strong acid as a catalyst, which causes problems such as reaction equipment corrosion, environmental pollution, and excessive unfavorable by-products for separation. [0003] The gas-phase synthesis method adopts an environmentally friendly solid catalyst, with CH 3 OH is used as an alkylating agent to catalyze the synthesis of N-methylaniline from aniline under gas phase conditi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J23/86C07C209/18C07C211/48
CPCB01J21/04B01J23/005B01J23/868B01J27/24C07C209/18C07C211/48
Inventor 吕新宇邱滔石伟红沈益秀
Owner CHANGZHOU UNIV
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