Patent GB-383148-A (GB)
Title: Improved process of dehydrating aqueous acetic acid
IPC: C07C51/46
Filed: 1932-03-16
Abstract: <PICT:0383148/IV/1> <PICT:0383148/IV/2> Aqueous acetic acid is concentrated by distilling with propylene chloride.  The acid from a tank 6, Fig. 1, and propylene chloride from a tank 10 are supplied to a tall column 1 upon a still 2.  An azeotropic mixture is condensed at 13 and the propylene chloride layer is decanted at 15 and returned to the column.  Alternatively the acetic acid may be vaporized in a still 19, the vapour being admitted to the column 1; or the acetic acid may be admitted in both liquid and vapour form.  In any case concentrated acid collects in the still 2 and is withdrawn at 4.  In another arrangement, the aqueous acid from a tank 38, Fig. 2, is admitted to a column 41 upon a still 44, and propylene chloride is admitted to the column from a pipe 43 having a nozzle 42.  The azeotropic mixture condenses at 47, and the propylene chloride layer is decanted at 49 and returned to the column 41.  The aqueous layer is fed to a column 72 into which steam is admitted at 73.  The small quantity of propylene chloride is condensed at 75 and passes to the decanter 49.  The strong acid collecting in the still 44 is passed to a column 55 on a still 56 to remove remaining propylene chloride. The vapour is condensed at 59 and the condensate is passed in part to the column 41 and in part is returned to the column 55 to provide a reflux.  The concentrated acid from the still 56 may be taken to a simple still 67 to remove colouring or polymerized matter, pure acid being condensed at 70.  The process may also be effected by simple distillation with propylene chloride in a flask as a batch process.ALSO:Aqueous acetic acid is concentrated by distilling with propylene chloride.  The acid from a tank 6, Fig. 1, and propylene chloride from a tank 10 are supplied to a tall column 1 upon a still 2.  An azeotropic mixture is condensed at 13 and the propylene chloride layer is decanted at 15 and returned to the column. Alternatively the acetic acid may be vaporized in a still 19, the vapour being admitted to the column 1, or the acetic acid may be admitted in both liquid and vapour form.  In any case concentrated acid collects in the still 2 and is withdrawn at 4. In another arrangement, the aqueous acid from a tank 38, Fig. 2, is admitted to a column 41 upon a still 44, and propylene chloride is admitted to the column from a pipe 43 having a nozzle 42.  The azeotropic mixture condenses at 47, and the propylene chloride layer is decanted at 49 and returned to the column 41.  The aqueous layer is fed to a column 72 into which steam is admitted at 73.  <PICT:0383148/III/1> <PICT:0383148/III/2> The small quantity of propylene chloride is condensed at 75 and passes to the decanter 49.  The strong acid collecting in the still 44 is passed to a column 55 on a still 56 to remove remaining propylene chloride.  The vapour is condensed at 59 and the condensate is passed in part to the column 41 and in part is returned to the column 55 to provide a reflux.  The concentrated acid from the still 56 may be taken to a simple still 67 to remove colouring or polymerized matter, pure acid being condensed at 70. The process may also be effected by simple distillation with propylene chloride in a flask as a batch process.