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Method for preparing p-aminoanisole by catalytic hydrogenation

A technology of p-aminoanisole and p-nitroanisole, which is applied in the field of catalytic hydrogenation to produce p-aminoanisole, can solve the problems of high reaction temperature, long reaction time, complicated separation of reaction products and catalysts, and achieve The effect of stable catalyst performance and high strength

Inactive Publication Date: 2019-11-05
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the solvent and catalyst can be recycled, the method has higher reaction temperature, longer reaction time, and complicated separation of reaction product and catalyst.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 12.86g of Ni(NO 3 ) 2 .6H 2 O, 2.45g of Al(NO 3 ) 3 9H 2 O and 7.88g of Mg(NO 3 ) 2 ·6H 2 O was dissolved in 200ml of distilled water to obtain solution A, and 14.32g of anhydrous Na 2 CO 3 Dissolve in 200 ml of distilled water to obtain solution B. Under stirring conditions, solution A and solution B were added dropwise into 200ml of distilled water at the same time to form a green precipitate, and the filter cake obtained by washing and dehydrating the precipitate was dispersed in 200ml of n-butanol, and the solvent was evaporated at 353K, and continued at 393K drying to obtain a supported metal nickel catalyst precursor. The obtained catalyst precursor is pressed into tablets, sieved, and 20-40 mesh catalyst precursor particles are collected by sieving.

Embodiment 2

[0018] Take 10 g of the catalyst precursor particles in Example 1, fill them into the reaction tube of the reduction passivation device, and reduce them at 723 K for 2 hours in 40 ml / min flowing hydrogen, and then lower the temperature to room temperature. The hydrogen flow was stopped and replaced with nitrogen flow. A small amount of air was then added to the nitrogen stream to passivate the catalyst. Slowly increase the air flow until the temperature rise no longer occurs, which means that the passivation is completed and a pre-reduced metal nickel catalyst is obtained.

[0019] Example 2

[0020] Take 2g of the pre-reduced metal nickel catalyst particles prepared in Example 2, fill them into a fixed-bed reaction tube, activate them at 523K for 2 hours in 40ml / min flowing hydrogen, and then cool down to 333K. The hydrogen pressure was raised to 2.0 MPa, and the N,N-dimethylformamide solution with a mass content of 10% p-nitroanisole was pumped into the reactor by a meteri...

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Abstract

The invention discloses a method for preparing p-aminoanisole by catalytic hydrogenation, and belongs to the technical field of catalytic hydrogenation. A p-nitroanisole solution is taken as a raw material, catalytic hydrogenation reaction is carried out in a trickle bed reactor by using a supported metallic nickel catalyst under a hydrogen atmosphere of 313-343 K and 1.0-2.0 MPa, on-line operation lasts for more than 4500 h, the conversion rate of the p-nitroanisole is greater than 99%, and the selectivity of the p-aminoanisole is greater than 99%.

Description

technical field [0001] The invention relates to a method for preparing p-aminoanisole by catalytic hydrogenation, which belongs to the technical field of catalytic hydrogenation. [0002] technical background [0003] P-aminoanisole is an important dye, spice and pharmaceutical intermediate. The traditional production process of p-aminoanisole is to use p-nitroanisole as raw material, and obtain p-aminoanisole through reduction with alkali sulfide or iron powder. The process technology is simple and mature, but the product quality is poor, the labor intensity is high, and the production cost is high. In particular, a large amount of industrial waste that is difficult to handle is produced as a by-product, which seriously pollutes the environment and human health. Therefore, many countries and regions have banned the use of traditional processes and turned to catalytic hydrogenation to produce p-nitroanisole. The product of catalytic hydrogenation process has high yield and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C217/84B01J23/755
CPCC07C213/02B01J23/78B01J23/002B01J2523/00C07C217/84B01J2523/22B01J2523/31B01J2523/847
Inventor 沈俭一倪自林傅玉川裴恒张家友
Owner NANJING UNIV
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