PATENT 3549. ----- [STANDARD OIL CO.] Separation of Oxygenated Organic Compounds by Distillation. British Patent 655,698, Sept. 15, 1948. British Abs., B, II, 1952, p. 4. Mixture of oxygenated compounds obtained during the Fischer-Tropsch synthesis or by oxidation of hydrocarbons is separated into components by distillation in presence of a large volume % of H2O. Thus, an aqueous layer containing alcohols 84.6, ketones and aldehydes 11.2, esters 0.2, and acids 4 mol.-% at 91° is passed at 485 cc. per hr. to the midpoint of a 1-in. diameter perforated plate column of 60 plates, while adding H2O at 94° to the top of the column at 945 cc. per hr. with overhead temperature 84° and reflux ratio 15:1:6.2% of material (ketones, aldehydes, esters) is collected as overhead and the bottoms fraction, comprising acids and alcohols, is passed at 91° into a 2d distillation zone at 1,310 cc. per hr. (reflux ratio 5:1). Alcohols are removed at 79° as overhead, and a solution of acids in H2O is withdrawn from the bottom and recycled to the 1st column. The feed may be initially distilled to separate it into 2 fractions, 1 within the range ofC1-2—C1-3 alcohols, and the other C3-5; both fractions are then subjected to extractive distillation as above. |