GB1205046A - Process for purifying adiponitrile - Google Patents

Abstract

1,205,046. Recovery and purification of adiponitrile. ASAHI KASEI KOGYO K.K. 16 Nov., 1967 [16 Nov., 1966], No. 62219/67. Heading C2C. [Also in Division C7] In a process for recovering adiponitrile from an adiponitrile-containing reaction mixture obtained in the electrolytic dimerization of acrylonitrile using a catholyte which is kept in an emulsion state and which contains a supporting electrolyte, the emulsified catholyte (if desired after allowing it to settle out into two phases, i.e. an oil phase and an aqueous phase, removing a part of the aqueous phase thus separated therefrom, and recombining the oil phase and the remaining aqueous phase) is distilled in an acrylonitrile rectifying tower to remove a part of the acrylonitrile and water therefrom and the residue obtained is separated into two phases, i.e. an oil phase and an aqueous phase, and adiponitrile is recovered from the oil phase thus separated, the supporting electrolyte being capable of separating the concentrated residue obtained by distillation of catholyte into the two phases. The aqueous phase component separated from the residue in the acrylonitrile rectifying tower may be recycled to the catholyte tank, while the oil phase component comprising adiponitrile, water and a supporting electrolyte may firstly be extracted with water and/or a saturated solution of acrylonitrile and the adiponitrile subsequently recovered by charging said oil phase to a lower boiling component separator from the top of which a distillate comprising water, acrylonitrile and ethylene cyanohydrin is obtained and from the bottom of which is obtained a residue comprising adiponitrile and also, as impurities, biscyanoethyl ether and acrylonitrile oligomer, which residue is charged to an adiponitrile rectifying tower from the top of which purer adiponitrile is distilled and from the bottom of which is obtained a residue comprising adiponitrile, biscyanoethyl ether and acrylonitrile oligomer which is charged to an adiponitrile stripper, the vapour from the top of which is supplied to the lower boiling component separator, leaving a liquid residue of acrylonitrile oligomer, biscyanoethyl ether and supporting electrolyte which is withdrawn. As an alternative the whole of the distillate from the acrylonitrile rectifying tower may be supplied to a propionitrile separator in which propionitrile and water are left as a residue as acrylonitrile and water are distilled off, the acrylonitrile being recycled to the catholyte tank. The supporting electrolyte in the catholyte employed should be capable of separating the concentrated residue obtained by distillation of catholyte consisting of the oil and aqueous phases into two phases and may be, for example, a sulphate, halide, monomethyl sulphate or monoethyl sulphate which contains as cation a quaternary ammonium, ammonium or alkali metal ion. Other conventional additives may be present and a suitable flow diagram for the process is described.