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Preparation method of 2,4-diaminophenyl methyl ether

A technology of diaminoanisole and dinitroanisole, which is applied in the field of preparation of 2,4-diaminoanisole, and can solve problems such as environmental pollution, low product purity or production capacity, and many wastes

Inactive Publication Date: 2018-06-29
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 that the existing 2,4-diaminoanisole preparation method has harsh reaction conditions, severe equipment corrosion, many wastes, serious environmental pollution or low catalyst recycling rate, cannot be continuously produced, and the product Purity or production capacity are low defects, and a kind of preparation method of 2,4-diaminoanisole is provided

Method used

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  • Preparation method of 2,4-diaminophenyl methyl ether

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Effect test

Embodiment 1

[0095] A kind of preparation method of 2,4-diaminoanisole, take 2,4-dinitroanisole 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 2,4-diaminoanisole.

[0096] Specific steps include:

[0097] (1) Put 5000kg of methanol and 1250kg of 2,4-dinitroanisole into the chemical material tank, follow-up feeding is carried out according to the ratio, stir evenly, pump into the first-level 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 2,4-dinitroanisole is passed...

Embodiment 2

[0101] (1) Put 5000kg of methanol and 1250kg of 2,4-dinitroanisole 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 2,4-dinitroanisole 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, the material stays in the hydrogenation kettle for about 2-3h, and the reaction is...

Embodiment 3

[0105] (1) 12500kg of methanol and 1250kg of 2,4-dinitroanisole 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 2,4-dinitroanisole 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, the material stays in the hydrogenation ke...

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Abstract

The invention discloses a preparation method of 2,4-diaminophenyl methyl ether. The preparation method comprises the steps of carrying out continuous catalytic hydrogenation on 2,4-dimitroanisole, andthen carrying out sedimentation and membrane filtration to obtain the 2,4-diaminophenyl methyl ether. The method is simple to operate and high in safety, can realize continuous production, is high inproduction efficiency, high in product quality, low in labor intensity, environmentally-friendly and high in catalyst utilization rate, and has an effect of being beneficial to industrialization.

Description

technical field [0001] The invention relates to a preparation method of 2,4-diaminoanisole. Background technique [0002] 2,4-Diaminoanisole (DAA for short) is an important fine chemical intermediate, which is mainly used in chemical production processes such as dyes, medicines, and pesticides. The preparation of 2,4-diaminoanisole usually uses 2,4-nitroanisole as a raw material, and it is prepared by reducing sodium sulfide or iron powder. The traditional process consumes a lot of materials and discharges waste water and residue, which will cause Serious environmental pollution. The preparation of 2,4-diaminoanisole by catalytic hydrogenation of 2,4-dinitroanisole is a green process route for the synthesis of aromatic amino compounds, but the existing catalytic hydrogenation method has catalyst separation and recovery issues such as low utilization. [0003] Therefore, how to provide a method for preparing 2,4-diaminoanisole with high production efficiency, high product ...

Claims

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Application Information

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IPC IPC(8): C07C213/02C07C213/10C07C217/84
CPCC07C213/02C07C213/10C07C217/84Y02P20/584
Inventor 刘云龙曲美君戴杰张永明杨勇
Owner YANTAI ANOKY FINE CHEM CO LTD
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