Preparation method of m-phenylenediamine

A technology for m-phenylenediamine and m-dinitrobenzene is applied in the field of preparation of m-phenylenediamine, and can solve the problems of many three wastes, harsh reaction conditions of m-phenylenediamine, serious equipment corrosion, etc.

Inactive Publication Date: 2018-06-15
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

[0003] The technical problem to be solved by the present invention is that the existing m-phenylenediamine preparation method has harsh reaction conditions, serious equipment corrosion, many wastes, serious environmental pollution, low catalyst recycling rate, inability to continuously produce, and low product purity or production capacity, etc. defect, and a kind of preparation method of m-phenylenediamine is provided

Method used

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  • Preparation method of m-phenylenediamine

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Effect test

Embodiment 1

[0094] A kind of preparation method of m-phenylenediamine, take m-dinitrobenzene as raw material, adopt Pd / Al 2 o 3 Catalyst, continuous catalytic hydrogenation reaction is carried out in the reactor, after the catalyst is separated and recovered, the reducing solution is desolvated and purified to obtain the target product m-phenylenediamine.

[0095] Specific steps include:

[0096] (1) Put 5000kg of methanol and 1250kg of m-dinitrobenzene into the chemical tank, follow-up feeding according to this ratio, stir evenly, pump them 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 m-dinitrobenzene is passed into H 2 , control the...

Embodiment 2

[0100] (1) Put 5000kg of methanol and 1250kg of m-dinitrobenzene into the chemical material tank, and follow up the ratio of feeding materials, stir evenly, pump them into the primary 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 m-dinitrobenzene 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 reac...

Embodiment 3

[0104] (1) 12500kg of methanol and 1250kg of m-dinitrobenzene are put into the chemical tank, and the subsequent feeding is stirred evenly according to the ratio, and evenly stirred, 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 m-dinitrobenzene 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 kettl...

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Abstract

The invention discloses a preparation method of m-phenylenediamine. M-dinitrobenzene is subjected to continuous catalytic hydrogenation, settlement and membrane filtration, and m-phenylenediamine is obtained. The method is simple to operate and high in safety, can be used for continuous production, can achieve the effects of high production efficiency, high product quality, low labor intensity, environmental friendliness and high utilization rate of a catalyst, and is beneficial to the effect of industrialization.

Description

technical field [0001] The invention relates to a preparation method of m-phenylenediamine. Background technique [0002] m-Phenylenediamine is an important raw material for organic synthesis, mainly used as a dye intermediate for the manufacture of basic orange, basic brown G, direct fast black G and other dyes, and as fur dyes. It is an important intermediate for the production of pesticides, medicines, and functional materials. It is used as a curing agent for epoxy resins, as a coagulant for cement, as a mordant, and as a color developer, as well as as a raw material for petroleum additives and pharmaceuticals. , as a photometric reagent for the determination of nitrite and active chlorine in water. In the past, the method of producing m-phenylenediamine basically used iron powder reduction or alkali sulfide reduction process. These two reduction processes will produce a large amount of three wastes, and the product quality is poor and the yield is low. In recent years,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/36C07C209/86C07C211/51
CPCC07C209/36C07C209/86C07C211/51Y02P20/584
Inventor 辛森森刘云龙曲美君张永明戴杰
Owner YANTAI ANOKY FINE CHEM CO LTD
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