VERFAHREN ZUR DESTILLATIVEN REINIGUNG VON ROHEM SEC-BUTYLALKOHOL.

摘要

Continuous distillative purifcn. of crude sec.-BuOH(SBA), obtd. by catalytic hydration of n-butene at elevated temp. and elevated pressure and sepn. of unreacted olefin from the reaction prods., involves passing crude SBA into the upper pt. of a sepg. column, supplying the energy needed for vapourisation through a reboiler at the bottom of the sepg. column, distilling off the azeotropic and light (low boiling) by-prods. at the top, discharging the prepurified SBA from the sump of the sepg. column and then sepg. the heavy (high boiling) by-prods. The novelfeatures are that: a) practically anhydrous crude SBA is purified by supplying the amt. of water needed for the azeotropic compsn. of the top prod. to the top plate of the sepg. column and removing the added water from this plate upwards by applying a standard temp. of 87.5-99.5 deg.C at the middle plate; c) the crude SBA is supplied to a plate just below the top of the folumn, apolar light by-prods. are expelled azeotropically as ternary azeotrope with SBA and water by extractive distn. in the zone contg. water, between the supply plate and heated plate, whilst polar by-prods. are expelled between the heated plate and sump conc. by rectification in the zone between the supply plate and top; the distn. prod. from the top is condensed and the resultant 2 phases are recycled to a stream directly from the bottom of the reflux vessel to the top plate of the sepg. column and only the increase in light phase obtd. due to distn. of the crude SBA is discharged as by-prod. stream; and fresh water is used to maintain the required azeotropic compsn. of the top prod. and replace the water discharged in theby-prod. stream and this is applied with the 2-phase reflux to the top plate of the sepg. column, the fresh water supply being regulated according to the top temp. of the sepg. column.