Abstract:
1,218,706. Separation of nitroalkanes and alkanes. COMMERCIAL SOLVENTS CORP. 9 July, 1969 [26 Aug., 1968], No. 34622/69. Heading C2C. [Also in Division C5] A mixture of one or more nitroalkanes having 2 to 4 carbon atoms and one or more alkanes (including cycloalkanes) having 5 to 9 carbon atoms is separated by (a) adding methanol to the mixture in an amount sufficient to initiate co-distillation with the alkane or alkanes when said mixture is heated, (b) heating and codistilling the alkane-methanol thereby effecting separation of the alkane or alkanes and producing a residue of nitroalkane or nitroalkanes and methanol, and (c) separating the methanol from the nitroalkane or nitroalkanes. The alkanemethanol distillate may be condensed into two layers, and the lower methanol layer returned to the distillation unit until alkane no longer comes over in the distillate. The upper alkane is suitable for re-use without further treatment or it can be freed from methanol by distillation or washing with water.
Abstract:
Congo red is removed from an aqueous solution thereof by immersing in the solution an inclusion resin made by cross-linking cyclodextrin with epichlorohydrin. The congo red is absorbed on the resin.ALSO:A water-insoluble inclusion resin, having the property of forming inclusion complexes with organic and inorganic substances, is based on cyclodextrin. The resin may be made by cross-linking alpha-, beta- or gamma-cyclodextrins with e.g. epichlorohydrin, dichlorohydrin, diepoxybutane, diepoxy-propyl ether, ethylene glycol diepoxy-propyl ether or formaldehyde, or by embedding the cyclodextrin in a water-insoluble polymer such as polyamide, polyvinyl acetal, epoxy resin, nitrocellulose, acetyl cellulose, ethyl cellulose, polyacrylamide, polymethacrylamide, polyacrylate or polymethacrylate. Cross-linking may be effected in acid or alkaline, aqueous or non-aqueous media depending upon the reagents and the properties desired in the product, and may be carried out under an inert gas. Embedding the cyclodextrin may be carried out by dispersing it in a solution of polymer, and then removing the solvent, or by polymerizing a monomer containing dispersed cyclodextrin. The inclusion resin may be subjected to further modification. For example, the resin may be oxidized, with conversion of secondary hydroxyl groups to aldehyde groups, and the oxidized resin then treated with hydroxylamine to form oxime-type products, or reduced by sodium borohydride or lithium aluminium hydride, or further oxidized to form carboxyl groups. In examples (1) cyclodextrin is cross-linked by epichlorohydrin; (2) cyclodextrin is cross-linked by formaldehyde; (3) a dispersion of cyclodextrin in an acetone solution of acetyl cellulose is evaporated. In further examples, the inclusion resins are used to remove Congo red, o-nitrophenol, and benzaldehyde from aqueous solutions thereof, and to separate mixtures of inorganic and organic compounds. Example 11 relates to the oxidation ofcyclodextrin cross-linked by epichlorohydrin by periodate to form a dialdehyde derivative.ALSO:An inclusion resin made by cross-linking cyclodextrin with epichlorohydrin is used to separate (1) o-nitrophenol and p-nitrophenol; (2) phenylalanine and tryptophane; (3) p-nitrophenol, or o-nitrophenol or benzaldehyde from aqueous solutions thereof. Mixtures (1) and (2) are eluted from a column of the inclusion resin, one component being preferentially absorbed, while the organic compounds (3) are absorbed on powdered resin immersed in the aqueous solutions.
Abstract:
Nitromethane is recovered from mixtures with higher nitroalkanes by adding to said mixtures sufficient water and C6- 8 alkane or cycloalkane to form an azeotropic mixture with said nitromethane, and heating the mixture to distil off said azeotrope. The said azeotrope condenses into three layers, the lowest of which contains the nitromethane with minor amounts of water and alkane. The water and alkane may be removed by further distillation up to 101.5 DEG C.
Abstract:
A process for the continuous separation of nitrocyclohexane from the gaseous products of cyclohexane vapour-phase nitration comprises partial condensation of said products, removal of fatty acids from the condensate by alkali washing, distillation to remove cyclohexane and water and further distillation-at sub-atmospheric pressure-of the nitrocyclohexane. The latter may be further purified by steam distillation, preferably in presence of a surface-active agent.