Reaktion #355149
ord-18ae49017b5f4435968b06dc2cb2ebea
Reaktionsgleichung
Reagenzien
Reaktionsbedingungen
Aufarbeitung
- 1workup.ADDITIONwere mixed together
Vorschrift
An aqueous 6% aluminum nitrate solution containing 324 g of aluminum nitrate, Al(NO3)3.9H2O and an aqueous 15% sodium silicate solution containing 356 g of silicon oxide were mixed together to form a slurry of aluminum hydroxide and silicic acid gel. The resulting slurry mixture was washed with water until there was no soluble salt contained therein, and dried at 110°C under aeration. 400 Grams of the thus obtained pellets having a ratio of silica to alumina of 89:11 by weight and having particle sizes of 3 mm was immersed in 800 g of an aqueous 5% ammonium iodide solution at room temperature, for example, 25° to 30°C, for 4 days, then thoroughly washed with water to remove iodine ions, and dried at 120°C. 500 ml of the thus prepared silica-alumina catalyst was filled in a tubular reactor, and a gas mixture consisting of 12 moles of formaldehyde, 12 moles of acetaldehyde and 26.4 moles of ammonia preheated to 200°C was passed through the tubular reactor for 3 hours (SV = 1,160 hr-1), while keeping the tubular reactor at 420°C. The reaction gas mixture passed through the catalyst layer was cooled, and subjected to condensation. The resulting condensate was dehydrated with caustic soda, and 492 g of the thus obtained oil was distilled and quantitatively determined by gas chromatograph. The yields of the thus obtained reaction products were 38.1% pyridine (2.74 moles), 25.9% 3-picoline (1.55 moles) and 3.3% 3,5-lutidine (0.17 mole) on the basis of the amount of carbon of the aldehyde used. After the completion of the reaction, the catalyst was regenerated by burning the carbons deposited on the catalyst with air at 560°C or less. The required regeneration time was 3 hours.