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公开(公告)号：US3177235A
公开(公告)日：1965-04-06
申请号：US28251663
申请日：1963-05-22
申请人： LABOFINA SA
CPC分类号： C07F15/045 , B01J31/1805 , B01J2531/847 , C07C7/152 , C08F4/06 , C07C15/02 , C07C15/00
摘要： The invention comprises a Werner complex of 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 in which R1 is either hydrogen or a primary alkyl group and R2 is a phenyl group carrying two further halogen substituents on the 3- and 4-positions, and n is either 2 or 4. R1 preferably contains 1 to 10, more particularly 1 to 6, carbon atoms. The halogen substituents are conveniently identical and may be chlorine or bromine. The complexes are made, according to an 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. Specific examples of amines are a (3,4-dichlorophenyl) ethylamine, a (3,4 - dichlorophenyl) butylamine, a (3,4 - dichlorophenyl) heptylamine, a (3,4 - dibromophenyl) ethylamine. They may be prepared by reductive amination of the corresponding ketones, for instance by heating with ammonium formate. Specifications 931,775, 935,099, 937,791 and 945,012 are referred to.ALSO:Clathrates of aromatic hydrocarbons are made using a Werner complex of the general formula Ni(SCN)2Xn, wherein X is an alpha-arylalkylamine of the formula in which R1 is either hydrogen or a primary alkyl group and R2 is a phenyl group carrying two halogen substituents on the 3- and 4-positions, and n is 2 or 4. The clathrates may be made heating a complex Ni(SCN)2X4 with one or more clathratable aromatic hydrocarbons to a temperature at which all the complex is dissociated into Ni(SCN)2X2 and 2X, and then cooling to effect recombination of the components to form the clathrate. Alternatively a complex Ni(SCN)2X2, at least two motor equivalents of amine X and at least one clathratable aromatic hydrocarbon are mixed together to form a clathrate in which the complex is Ni(SCN)2X4. A mixture of aromatic hydrocarbons containing at least one such clathratable compound can be resolved by forming a clathrate with a complex of the type Ni(SCN)2X4 and the clathratable compound or compounds in the mixture, separating the clathrate from the mixture and dissociating the clathrate, e.g. by heating, treatment with an acid which does not react with the clathrated compounds, steam stripping or elution with an inert solvent. In examples, isomers of di-isopropylbenzenes, cymenes, ethylisopropylbenzenes, cyclohexyltoluenes, and methylnaphthalenes are separated. Specifications 931,775, 935,099, 937,791 and 945,012 are referred to.
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2.发明授权Separation of aromatic compounds by forming clathrates with werner complexes of 2-arylalkylamines 失效通过与2-芳基烷基胺的维纳络合物形成包合物来分离芳族化合物
公开(公告)号：US3177266A
公开(公告)日：1965-04-06
申请号：US28242963
申请日：1963-05-22
申请人： LABOFINA SA
IPC分类号： B01J31/18 , C07C7/152 , C07C17/38 , C07C201/16 , C07F15/04
CPC分类号： C07F15/045 , B01J31/1805 , B01J2531/847 , C07C7/152 , C07C17/395 , C07C211/27 , C07C15/00 , C07C15/02 , C07C25/08 , C07C25/10 , C07C22/08
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 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.
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公开(公告)号：US3076005A
公开(公告)日：1963-01-29
申请号：US17676462
申请日：1962-03-01
申请人： LABOFINA SA
CPC分类号： B01J31/1805 , B01J2531/847 , C07F15/045
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公开(公告)号：US3177234A
公开(公告)日：1965-04-06
申请号：US28223163
申请日：1963-05-22
申请人： LABOFINA SA
IPC分类号： B01J31/18 , C07C7/152 , C07C17/38 , C07C201/16 , C07F15/04
CPC分类号： C07F15/045 , B01J31/1805 , B01J2531/847 , C07C7/152 , C07C17/395 , C07C211/27 , C07C15/00 , C07C15/02 , C07C25/08 , C07C25/10 , C07C22/08
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 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.
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