Patent GB-958828-A (GB)
Title: Purification of synthetic methanol
IPC: C07C31/04
Filed: 1962-09-04
Abstract: 958,828. Purification of methanol by distillation. CHEMICAL CONSTRUCTION CORPORATION. Sept. 4, 1962 [Sept. 8, 1961], No. 33816/62. Heading BIB. Crude synthetic methanol is purified from high boiling and low boiling impurities by extractive distillation with water to produce a bottoms stream of aqueous methanol, followed by the fractional distillation of this stream to yield anhydrous methanol; the extractive distillation stage being characterized by the removal of a liquid side stream comprising high boiling impurities and some methanol from the middle section of the column, the extraction of this side stream with water to remove a portion of the high boiling impurities as a waterimmiscible phase, and the recycling of the aqueous phase back into the middle section of the column. The feed of crude methanol flowing in line 1 is mixed with recycle streams flowing in lines 2, 3 and 4, and the combined feed stream enters extractive distillation column 8 via line 5, heat exchanger 6 and line 7. Water at a temperature of 85-125 ‹F. is added via line 9. Preferably this water is maintained slightly alkaline in pH in order to liberate any ammonia, and to neutralize any carboxylic acid, present in the feed. The vapour stream leaving column 8 via line 10 contains practically all the low boiling impurities, water vapour, a small proportion of methanol and traces of the high boiling impurities. This vapour stream is partially condensed in condenser 11, part of the condensate being returned as reflux to the column via line 15, the remainder being discarded via line 16. The vapour stream 13 is either discarded or further cooled in unit 17 to obtain a product stream of dimethyl ether via line 19, and a residual vapour stream 20 which is discarded. Side streams 21 and 22 are withdrawn from the central section of column 8, to form a composite stream 23 which is cooled to a temperature of 75-140 ‹F. in cooler 24. The cooled stream 25 is extracted with water in the extractor-decanter unit 26, the water being introduced via line 27. The extract separates into a water-immiscible phase containing a portion of the high boiling impurities, and an aqueous phase containing the methanol and the remaining high boiling impurities. The waterimmiscible phase is discarded via line 28, and the aqueous phase is recycled to column 8 via line 2. Purified aqueous methanol, containing traces of organic impurities, is removed from the base of column 8, heated to 205-220 ‹F. in heat exchanger 31, and passed into distillation column 33. Fractional distillation of the aqueous methanol takes place to yield a highly purified anhydrous methanol product which is withdrawn as a liquid phase from the top section of the column via line 36. Final purification of this methanol stream is obtained by cooling it in cooler 37 and passing it through a bed 39 of activated carbon. The vapour withdrawn from the top of the column 33, comprising residual low boiling impurities and some methanol, is condensed in condenser 42, part of the condensate being returned to column 33 as reflux, the remainder being recycled to the primary feed to column 8 via line 4. Residual high boiling impurities are withdrawn from column 33 via the side streams 45 and 46, and are returned to the primary feed to column 8 via line 3. Water, free from methanol, is withdrawn as the bottoms product from column 33. The second column may be operated at an elevated pressure, so that the vapour withdrawn from the head of the column can be used as the heat source for the reboiler section of the extractive distillation column. Specification 660,773 is referred to.