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Preparation method of P-aminoanisole

A technology for p-aminoanisole and p-nitroanisole is applied in the field of preparation of p-aminoanisole, and can solve the problems of environmental pollution, low catalyst recovery rate, low product purity and the like

Inactive Publication Date: 2018-06-08
YANTAI ANOKY FINE CHEM CO LTD +4
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the problems of serious environmental pollution, low catalyst recycling rate, low product purity or low production capacity in the preparation process of p-aminoanisole in the prior art, thereby providing a kind of The preparation method of aminoanisole

Method used

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  • Preparation method of P-aminoanisole

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Effect test

Embodiment 1

[0095] A kind of preparation method of p-aminoanisole, take p-nitroanisole as raw material, adopt Pd / Al 2 o 3 The catalyst is used for continuous catalytic hydrogenation reaction in the reactor. After the catalyst is separated and recovered, the reducing solution is desolvated and purified to obtain the target product p-aminoanisole.

[0096] Specific steps include:

[0097] (1) Put 5000kg of methanol and 1250kg of p-nitroanisole into the chemical tank, follow-up feeding according to this ratio, stir evenly, pump into the first-stage hydrogenation reactor, and add Pd / Al 2 o 3 Catalyst 125kg, the particle size of the catalyst is 10nm, pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 90-100°C, and pump it into the first-stage hydrogenation tank at a flow rate of 6000L / h The raw material solution of p-nitroanisole is passed into H 2 , control the hydrogen pressure ...

Embodiment 2

[0101] (1) Put 5000kg of methanol and 1250kg of p-nitroanisole into the chemical material tank, and follow up the feeding according to the ratio, stir evenly, pump them into the first-stage hydrogenation reactor, and add Pd / Al 2 o 3 125kg of catalyst, the particle size of the catalyst is 500μm; pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 80-90°C, and pump it into the first-stage hydrogenation tank at a flow rate of 5000L / h The raw material solution of p-nitroanisole is passed into H 2 , control the hydrogen pressure in the system to 3.0MPa, and add Pd / Al to the primary hydrogenation reactor every 3h 2 o 3 Catalyst 2.5kg, after the material in the primary hydrogenation kettle gradually increases, it flows into the secondary hydrogenation kettle through the overflow port, and the residence time of the material in the hydrogenation kettle is about 2-3h, and the ...

Embodiment 3

[0105] (1) 12500kg of methanol and 1250kg of p-nitroanisole are put into the chemical material tank, and the subsequent feeding is stirred evenly according to the ratio. After stirring evenly, it is pumped into the first-stage hydrogenation reactor, and Pd / Al is added. 2 o 3 Catalyst 125kg, the particle size of the catalyst is 10nm; pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 90-100°C, and pump it into the first-stage hydrogenation tank at a flow rate of 6000L / h The raw material solution of p-nitroanisole is passed into H 2 , control the hydrogen pressure in the system to 3.0MPa, and add Pd / Al to the primary hydrogenation reactor every 3h 2 o 3 Catalyst 2.5kg, after the material in the primary hydrogenation kettle gradually increases, it flows into the secondary hydrogenation kettle through the overflow port, and the residence time of the material in the hydr...

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Abstract

The invention discloses a preparation method of P-aminoanisole. The p-aminoanisole is obtained through performing continuous catalytic hydrogenation on paranitroanisole and then sedimentation and membrane filtration. The preparation method disclosed by the invention can achieve the effects of high production efficiency, high product quality, low labor intensity, environmental friendliness, high catalyst utilization rate and beneficial industrialization.

Description

technical field [0001] The invention relates to a preparation method of p-aminoanisole. Background technique [0002] 4-Aminoanisole is an important fine chemical intermediate, mainly used in the pharmaceutical and dye industries. Due to the wide range of uses of the product, the demand at home and abroad is relatively large. At present, the methods for producing p-aminoanisole include iron powder reduction, sodium sulfide reduction, hydrogenation reduction and p-hydroaniline method, etc. And industrial production mainly still adopts sodium sulfide reduction method to prepare p-aminoanisole, but this method pollutes the environment seriously; However, there are problems such as low catalyst separation recovery utilization rate. [0003] Therefore, how to provide a method for preparing p-aminoanisole with high production efficiency, high product quality, low labor intensity and environmental friendliness is a technical problem urgently needed by those skilled in the art. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C215/76
CPCC07C213/02C07C215/76Y02P20/584
Inventor 贺晓丽刘云龙曲美君张永明杨勇
Owner YANTAI ANOKY FINE CHEM CO LTD
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