Method for preparing p-aminodiphenylamine
A technology of p-aminodiphenylamine and nitrodiphenylamine, which is applied in the field of preparation of p-aminodiphenylamine, can solve problems such as difficult solvent recovery, long hydrogenation time, and hydrogenation of azobenzene, so as to avoid the control of moisture content, Simple operation and improved reaction efficiency
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[0029] Example 1. Pre-treat 50g of powdered activated carbon, soak in 200g of 3% nitric acid solution at 30°C for 8 hours, wash with deionized water to neutrality, then soak in 3% hydrogen peroxide solution for 4 hours, wash, and dry at 105°C for 16 hours.
[0030] Take 20g of treated activated carbon for later use. Dissolve a certain amount of palladium chloride and lanthanum nitrate in 100mL of 2% hydrochloric acid solution, pour them into a container with carrier activated carbon, stir for 4h, take it out, add 10mL of 5% formaldehyde for reduction, use 5% sodium hydroxide The pH of the solution is adjusted to 6-8, maintained for 4 hours, taken out, washed with deionized water, and vacuum dried at 80°C for 8 hours to obtain a catalyst product, which is recorded as Cat1.
Example Embodiment
[0031] Example 2. Pre-treat 50g of powdered activated carbon, soak in 200g of 3% hydrochloric acid solution at 60°C for 8 hours, wash with deionized water to neutrality, then soak in 5% hydrogen peroxide solution for 4 hours, wash, and dry at 105°C for 16 hours.
[0032] Take 20g of treated activated carbon for later use. Dissolve a certain amount of palladium nitrate and cerium nitrate in 100ml of 2% nitric acid solution, pour them into a container with carrier activated carbon, stir for 5h, take out, add 10ml of 5% hydrazine hydrate for reduction, use 5% sodium hydroxide The pH of the solution is adjusted to 6-8, maintained for 4 hours, taken out, washed with deionized water, and vacuum dried at 80°C for 8 hours to obtain a catalyst product, which is recorded as Cat2.
Example Embodiment
[0033] Example 3-6. The catalyst was prepared according to the method of Example 1, and the content of each component is shown in the table.
[0034] Table 1 The content of each component in the catalyst
[0035] Example catalyst palladium Rare earth elements 1 Cat1 5% (added as palladium chloride) La (added as lanthanum nitrate) 0.05% 2 Cat2 7% (added in the form of palladium nitrate) La (added in the form of lanthanum chloride) 0.70% 3 Cat3 9% (added as palladium acetate) Ce (added in the form of cerium chloride) 0.18% 4 Cat4 11% (added as palladium chloride) Pr (added as praseodymium chloride) 0.33% 5 Cat5 13% (added in the form of palladium nitrate) Nd (added as neodymium chloride) 0.65% 6 Cat6 15% (added in the form of palladium acetate) Sm (added as samarium chloride) 0.90%
[0036] The foregoing Examples 1-6 are the preparation of hydrogenation catalysts.
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