Improvements in the treatment of solids

摘要

Solid substances which per se would be solid at the distillation temperature employed are distilled by suspending or dissolving the solid in a liquid medium and submitting the suspension or solution to evaporative distillation at suitable temperatures under a vacuum of the order of 10<-2> to 10<-5> mm. of mercury. The process may be applied to the isolation or concentration of solid ingredients of plants, herbs, or animal substances, e.g. the distillation of caffeine from tea or coffee suspended in oil. Solid dyestuffs or intermediates may be isolated from solid mixtures containing them, madder may be distilled from madder root ground in oil, and solid impurities removed from phenol-aldehyde and other natural or synthetic resin suspensions. Examples are given of the purification of b -aminoanthraquinone and the o-anisidide of b -naphthoic acid. The distillation is preferably carried out by allowing the solution to flow from a conduit 5 in films over a vertical tube 3 internally heated by a resistance element 7. The distillate is condensed on the inner wall of a second tube 1 closely surrounding the tube 3 provided with pockets 2 for collecting fractions and cooled by water rings 8 and funnels 9. The condensates are led off to receivers 13 and the residue to a receiver 15.ALSO: Solid substances which per se would be solid at the distillation temperature employed are distilled by suspending or dissolving the solid in a liquid medium and submitting the suspension or solution to evaporative distillation at suitable temperatures under a vacuum of the order of 10<-2> to 10<-5> mm. of mercury. The process may be applied to the isolation or concentration of solid ingredients of plants, herbs, or animal substances, e.g. the distillation of caffeine from tea or coffee suspended in oil. Solid dyestuffs or intermediates may be isolated from solid mixtures containing them, madder may be distilled from madder root ground in oil, and solid impurities removed from phenol-aldehyde and other natural or synthetic resin suspensions. Examples are given of the purification of b -amino-anthraquinone and the o-anisidide of b -naphthoic acid. The distillation is preferably carried out by allowing the solution to flow from a conduit 5 in films over a vertical tube 3 internally heated by a resistance element 7. The distillate is condensed on the inner wall of a second tube 1 closely surrounding the tube 3 provided with pockets 2 for collecting fractions and cooled by water rings 8 and funnels 9. The condensates are led off to receivers 13 and the residue to a receiver 15. The Specification as open to inspection under Sect. 91 described the isolation of the female sex hormone by the distillation of finely divided placenta dispersed in oil. This subject-matter does not appear in the Specification as accepted.ALSO:The Specification as open to inspection under Sect. 91 described the isolation of the female sex hormone by the evaporative distillation under high vacua of finely divided placenta dispersed in oil. This subject-matter does not appear in the Specification as accepted.