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.
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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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