Patent GB-928777-A (GB)
Title: Process for separating acrylonitrile and ammonia from gaseous mixtures
IPC: B01D53/14
Filed: 1961-08-10
Abstract: <PICT:0928777/III/1> A process for separating acrylonitile and ammonia from gaseous mixtures comprises washing the said mixtures with liquids which preferentially absorb acrylonitrile, have dipole moment m  \sE 2,5D, dielectic constant e  \sE 10 (preferably \sE5), a ratio of Bunsen solubility coefficients at 20 DEG C. for acrylonitrile to ammonia of at least 10:1 (preferably at least 40:1) and a boiling range sufficiently remote from the boiling point of acrylonitrile to enable distillative separation. Specified washing liquids are liquid at a temperature about 20 DEG C., have a boiling point 110 DEG  to 280 DEG C., and are diphenyl, toluenes, xylenes, trimethyllbenzenes, cumene, prymene, 1,2,3,4 tetrahydronaphthalene, aliphatic hydrocarbons, decahydronaphthalene, a -methyl-naphthalene, a -ethyl naphthalene, anisole and diphenyl ether.  In one embodiment a eutectic mixture of diphenyl and diphenyl ether is used. The process is applicable to gases containing up to 20% by volume acrylonitrile and up to 50% by volume ammonia, or to the separation of acrylonitrile from practically pure ammonia.  As shown in the accompanying drawing, the starting gas mixture enters wash tower 3 by conduit 2, while wash liquid enters by conduit 4. The residual acrylonitrile-free wash gas escapes by outlet 5, while the washing liquid containing acrylonitrile and some ammonia is transferred by conduit 6 to the desorption column 7, the sump of which can be heated at 8 to promote expulsion of ammonia. An inert expelling gas, for example air, nitrogen, carbon dioxide or gaseous hydrocarbons, is introduced through conduit 9 and discharged through head outlet 11, while fresh washing liquid is supplied through conduit 10 to take up any desorbed acrylonitrile. The wash liquid is then transferred by outlet 12 to column 13 where it is washed with 2N sulphuric acid which removes the last traces of ammonia.  The wash liquid is then transferred via conduit 15, reservoir 17, pre-heater 18 and conduit 19 to distillation column 20.  Acrylonitrile is withdrawn via head outlet 22, while the wash liquid is removed via outlet 27 and recycled to columns 3 or 7. In one embodiment the washing column and the desorption column are combined in one stage, the former above the latter.  In another embodiment column 13 is omitted. Ammonia is subsequently separated from the acrylonitrile-free mixture by known means, e.g. washing with water.  Liquid entrained by the gas leaving the washing and desorption columns is recovered by known means, e.g. by adsorption on active carbon or by washing with heavy oil.  In embodiments wherein the gas mixture contains a gas such as acetonitrile, this will be separated out with the acrylonitrile.ALSO:A process for separating acrylonitrile and ammonia from gaseous mixtures, obtained for example during the manufacture of acrylonitrile in the gaseous phase from propylene and ammonia in the presence of air or oxygen, comprises washing the said mixtures with liquids which preferentially absorb acrylonitrile, have dipole moment m  \sE 2.5D, dielectric constant S  \sE 10 (preferably \sE 5), a ratio of Bunsen solubility coefficients at 20 DEG C. for acrylonitrile to ammonia of at least 10:1 (preferably 40:1) and a boiling range sufficiently remote from the b. pt. of acrylonitrile to enable distillative separation. Specified washing liquids are liquid about 20 DEG C., have a b. pt. 110 to 280 DEG C., and are diphenyl, toluene, xylenes, trimethylbenzenes, cumene, p-cymene, 1.2.3.4.tetrahydronaphthalene, aliphatic hydrocarbons, decahydronaphthalene, a  methyl naphthalene, a  ethyl naphthalene, anisole and diphenyl ether.  Examples are provided and apparatus for carrying out the process described (see Group III).