| 摘要 |
Oxygenated compounds, particularly aldehydes, are prepared by generating a "cobalt carbonyl," which term includes a carbonyl hydride, continuously subjecting carbon monoxide, hydrogen, and an olefin in the presence thereof to an OXO synthesis, and treating at least part of the product for recovery of cobalt; the generation and recovery operations each being effected in one of at least three separate zones, each of which is used in a cyclic sequence for generation and recovery, each when employed for generation containing a solid cobalt compound or cobalt metal on a solid support and being supplied with a gas comprising carbon monoxide, and each when employed for cobalt recovery containing a solid support and being supplied with at least part of the reaction product under conditions whereby the cobalt is deposited thereon. Preferably, each zone is used in sequence for catalyst generation, cobalt recovery, and treatment of recovered cobalt with hydrogen at 150-400 DEG C. The cobalt carbonyl may be formed by the action of carbon monoxide at a partial pressure of 20-300 atm. and at 30-250 DEG C. It may be prepared as a solution in, for example, hydrocarbons, alkanols or high boiling OXO products. Alternatively a gaseous product may be prepared and used as such or in solution. The OXO synthesis is preferably operated at 100-180 DEG C. and at least 50 atm. The weight of catalyst as cobalt may be .01-5 per cent. of the olefin. The product may be passed over a porous support, e.g. pumice, kieselguhr, silica gel or active charcoal, if desired with hydrogen, to recover the cobalt. For butyraldehyde, 150-200 DEG C. and 200-300 p.s.i. is suitable in this stage in absence of hydrogen. If the aldehyde is to be converted to alcohol, more drastic conditions such as hydrogen pressures up to 200 atm. or more may be used. With C2-C4 olefins, the aldehyde products may be flashed off and the residue subjected to cobalt recovery. Cobalt oxide may be used as the support whereon cobalt is deposited, reduction of the oxide and hydrogen treatment of the cobalt then being effected in one operation: water gas feed is passed through the catalyst generator, temperature and amount of feed being varied to control the amount of cobalt taken in to the reactor. When this falls too low, the generator is taken off stream and a second put on. OXO product passes to high and low pressure separators and then to the recovery vessel where cobalt is deposited until 15-20 per cent. by weight of the support when the stream is diverted to another vessel, the first being purged with inert-gas and then used as a catalyst generator. Specifications 631,316, 702,192, 702,221 and 702,241 are referred to. |
