Method for preparing 4-aminodiphenylamine
A technology of aminodiphenylamine and aniline, applied in the field of preparation of 4-aminodiphenylamine, can solve the problems of expensive catalyst, limited production scale, low product purity, etc., achieve high conversion rate and selectivity, reduce pollution, and make the preparation process continuous Effect
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Embodiment 1
[0038] Turn on the composite catalyst, aniline and nitrobenzene delivery pump at the same time, adjust the flow to 150 kg / h of aniline, 30 kg / h of nitrobenzene, and 100 kg / h of compound alkali catalyst, and continuously enter the forced heat exchanger for forced exchange. The heat medium of the heat exchanger is alcohol vapor, and the condensation liquid in the heat exchanger is forced to be pumped into the first-stage reactor from the top of the heat exchanger to continue dehydration and reaction, and then open the bottom valve of the first-stage reactor and the condensation circulation pump to adjust the outlet of the condensation circulation pump The valve returns the material to the forced heat exchanger to form a local circulation system, so that the material is continuously circulated, dehydrated and reacted. Control the reaction temperature at 75℃, the pressure (absolute pressure) at 0.008MPa, and control the circulating fluid flow at 2 meters 3 / hour. With the continuous e...
Embodiment 2
[0045] In a 500 ml three-necked flask equipped with a condenser and a stirrer, add 230 grams of water, add 91 grams of tetramethylammonium hydroxide (50%, 0.50 mol, the rest is water) and 20 grams of sodium hydroxide in an out of order (0.5 mol), 52 grams (0.25 mol) of tetramethyl ammonium carbonate, control the mixing temperature to 72-77 (°C), and stir evenly to obtain a composite alkali catalyst with a concentration of 29.9 (wt%).
Embodiment 3
[0047] Take 46 grams of nickel powder, 51 grams of aluminum powder, and 3 grams of copper powder, melt them in an induction furnace, discharging and cooling, and crush them into powder form, process, sieving, and keep the mesh number between 40-300 meshes. A 500 ml three-necked flask is equipped with a thermometer and a stirrer. 375 g of a 20% NaOH aqueous solution is charged. The powder is slowly added. The reaction temperature is maintained at 60°C and the reaction time is 4 hours. Then the catalyst is washed with water to Neutral, that is, a composite powder catalyst is obtained.
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