Separation of aromatic compounds by forming clathrates with werner complexes of 2-arylalkylamines,申请号US19630282429-传众专利搜索

Separation of aromatic compounds by forming clathrates with werner complexes of 2-arylalkylamines

申请公布号：US3177266(A)

申请号：US19630282429

申请日期：1963.05.22

申请公布日期：1965.04.06

申请人：

LABOFINA

发明人：PIERRE MARIE JOSEPH GHISLAIN DE RADZIT;HANOTIER JACQUES DANIEL VICTOR

分类号：B01J31/18;C07C7/152;C07C17/38;C07C201/16;C07F15/04

主分类号：B01J31/18

摘要：The invention comprises a Werner complex of the general formula Ni(SCN)2Xn which is insoluble or sparingly soluble, in water at room temperature, wherein X is an alpha-arylalkylamine of the formula <FORM:0994026/C2/1> in which R1 is either hydrogen or a primary alkyl group and R2 is a phenyl radical carrying at least two further alkyl substituents in any of the 3-, 4- and 5-positions, and n is either 2 or 4. Preferably R1 contains 1 to 6 carbon atoms and the alkyl substituents of the phenyl radical have not more than two carbon atoms. The complexes may be made, for example, by adding a solution of the arylalkylamine in heptane, or heptane-chloroform mixture, at room temperature to an aqueous solution obtained by dissolving NiCl2.6H2O and KSCN in water, and separating the resulting precipitate by filtration. The complexes may be used to form clathrates with aromatic compounds and the complex may be formed in the presence of the compound to be clathrated. The clathrate may be formed by heating a complex Ni(SCN)2X4 with one or more clathratable compounds to a temperature sufficient to bring about complete dissociation of the complex into Ni(SCN)2X2 and free amine, and then cooling to effect recombination of the dissociated components to form a clathrate consisting of Ni(SCN)2X4 and the clathratable compound. The complexes of the formula Ni(SCN)2X4 may be used to resolve a mixture of aromatic organic compounds containing at least one clathratable compound by forming a clathrate, separating the clathrate from the mixture and dissociating the clathrate to recover the organic compounds. The clathrate may be dissociated by heating, by treatment with an acid which does not react with the clathrated compound, by steam stripping or treatment with an inert solvent. Clathratable compounds which may be extracted or resolved are, for instance, a ,a ,a -tri -fluorotoluene, nitrobenzene, nitrotoluenes, di-, chlorobenzenes, trichlorobenzenes, cresols, and benzonitrile. Novel amines which are suitable for complex formation are a -(3,4-dimethyl phenyl) ethylamine and corresponding butylamine and heptylamine; a - (3,4,5 - trimethylphenyl) - ethylamine and - propylamine; a -(3,5 - dimethylphenyl) ethylamine and a -(3,4,5 - triethylphenyl) ethylamine. They may be made by reductive amination of the corresponding ketone, for example by heating the ketone with ammonium formate. Specifications 931,775, 935,099 and 945,012 are referred to.