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    Production of ethylenimine
    23.
    发明专利
    Production of ethylenimine 未知

    公开(公告)号：GB1062589A

    公开(公告)日：1967-03-22

    申请号：GB2710764

    申请日：1964-07-01

    Applicant: BASF AG

    Inventor： SINN RICHARD ,  SANNE WALTER ,  KINDLER HUBERT

    IPC: C07D203/08

    Abstract: The continuous production of ethylene-imine comprises mixing an aqueous alkaline solution of NH2CH2CH2OSO2OH (the alkali being in at least stoichiometric amount) with an amount of high-pressure steam to produce a temperature of 150 DEG to 300 DEG C., passing the mixture through a flow tube, and cooling to below 120 DEG C. by pressure release.

    Improvements in the separation of mixtures which contain a non-volatile complex catalyst
    26.
    发明专利
    Improvements in the separation of mixtures which contain a non-volatile complex catalyst 未知

    公开(公告)号：GB893809A

    公开(公告)日：1962-04-11

    申请号：GB557460

    申请日：1960-01-20

    Applicant: BASF AG

    Inventor： KINDLER HUBERT ,  TRIESCHMANN HANS GEORG

    IPC: C07C209/60

    Abstract: Mixtures, resulting from the synthesis of alcohols (from olefins, CO and H2O or of amines) (when part of the H2O is replaced by NH3 or primary or secondary amines), and containing a non-volatile complex catalyst formed by the reaction of an iron carbonyl, an amine, and H2O, are separated by treating with a stream of CO at elevated temperature to effect decomposition of the complex, removing condensable compounds from the CO stream, and rectifying the remaining mixture after recovery of the bulk of the iron as pentacarbonyl. The complex may be prepared from Fe(CO)4 or Fe(CO)6, and trimethylamine, N-butyl diethanolamine, pyrrolidine, piperidine, N-butyl piperidine, N-methyl pyrrolidine, or N-butyl-(3)-hydroxypyrrolidine. A nitrile, isonitrile, lactam, or sulphur compound containing a thioether bridge, or mixtures thereof (e.g. capronitrile, benzonitrile, adiponitrile, N-methyl pyrrolidone, caprolactam, caprylic lactam, thiodiglycol, or thiodibutyric acid) may be present in the complex-forming reaction mixture. The CO treatment may be at 70-130 DEG C. and atmospheric to 40 atmospheres. The Fe (CO)5 is separated from the other condensable constituents of the gas stream, which latter may be returned to the CO treatment. Thus, the gases may be passed up a column countercurrent to a reflux of the other condensable constituents, Fe(CO)5 separated from the condensate by decantation, and remaining gas returned to the reaction chamber. The CO may be mixed with inert gas, e.g. N2 or H2. After removal of Fe(CO)5 an aqueous base, e.g. caustic soda, may be added to the remaining mixture, before fractional distillation, to isolate acids. Syntheses referred to are propanol from ethylene, and butanol from propylene.ALSO:Mixtures, resulting from the synthesis of alcohols from olefins, CO, and H2O or of amines when part of the H2O is replaced by NH3 or primary or secondary amines, which contain a non-volatile complex catalyst formed by the reaction of an iron carbonyl, an amine, and H2O, are separated by treating with a stream of CO at elevated temperature of effect decomposition of the complex, removing condensable compounds from the CO stream, and rectifying the remaining mixture after recovery of the bulk of the iron as pentacarbonyl. The complex may be prepared from Fe(CO)4 or Fe(CO)6, and trimethylamine, N-butyl diethanolamine, pyrrolidine, piperidine, N-butyl piperidine, N-methylpyrrolidine, or N-butyl-(3)-hydroxy-pyrrolidine. A nitrile, isonitrile, lactam, or sulphur compound containing a thioether bridge, or mixtures thereof, e.g. capronitrile, benzonitrile, adiponitrile, N-methyl pyrrolidone, caprolactam, caprylic lactam, thiodiglycol, or thiodibutyric acid may be present in the complex-forming reaction mixture. The CO treatment may be at 70 DEG C.-130 DEG C. and atmospheric to 40 atmospheres. The Fe (CO)5 is separated from the other condensable constituents of the gas stream, which latter may be returned to the CO treatment. Thus, the gases may be passed up a column countercurrent to a reflux of the other condensable constituents, Fe(CO)5 separated from the condensate by decantation, and remaining gas returned to the reaction chamber. The CO may be mixed with inert gas, e.g. N2 or H2. After removal of Fe(CO)5 an aqueous base, e.g. caustic soda, may be added to the remaining mixture, before fractional distillation, to isolate acids. Syntheses referred to are propanol from ethylene, and butanol from propylene.

    Improvements in the production of alcohols and amines
    27.
    发明专利
    Improvements in the production of alcohols and amines 未知

    公开(公告)号：GB891067A

    公开(公告)日：1962-03-07

    申请号：GB1934160

    申请日：1960-06-01

    Applicant: BASF AG

    Inventor： KINDLER HUBERT ,  TRIESCHMANN HANS GEORG

    IPC: C07C209/60

    Abstract: A catalyst for use in the conversion of olefines, carbon monoxide and water to alcohols, and olefines, carbon monoxide, water and ammonia or primary or secondary amines to alkylated amines, comprises iron carbonyl and an amine, which form a complex in situ. Suitable amines for use in the catalyst are primary, secondary or tertiary amines either in the free state or as their salts. In the examples a catalyst consisting of N-n-butyl pyrrolidine and iron carbonyl is used for the production of butanol.ALSO:Alcohols or amines are formed by continuously reacting olefines, carbon monoxide and water or olefines, carbon monoxide, water and ammonia or a primary or secondary amine, respectively, at a temperature of 90 DEG C.-120 DEG C. and a carbon monoxide partial pressure of 2.0-7.0 atmospheres gauge, while using as catalysts complex iron carbonyl hydride compounds which are continuously formed during the reaction from iron pentacarbonyl and an amine. Under these conditions 12%-40% by weight of iron carbonyl compounds present are in the form of the pentacarbonyl. The iron carbonyl compound is usually added in the form of iron pentacarbonyl, but other carbonyls, e.g. the tetracarbonyl may be used. The process is used for the production of alcohols from olefines, carbon monoxide, e.g. propanol, butanol and pentanol and to the production of alkylated amines. Suitable primary and secondary amines for use in the production of alkylated amines are, for example, methylamine, dimethylamine, ethylamine, diethylamine, pyrrolidine, piperidine, aniline, p-phenylene diamine and also amines having additional functional groups, e.g. alanine, anthranilic acid and sulphanilic acid. In the examples propylene is reacted with carbon monoxide and water in the presence of iron carbonyl and N-n-butyl-pyrrolidine, to give butanol.

    Production of p-Dialkylbenzenes.
    28.
    发明专利
    Production of p-Dialkylbenzenes. 未知

    公开(公告)号：GB1170123A

    公开(公告)日：1969-11-12

    申请号：GB890267

    申请日：1967-02-24

    Applicant: BASF AG

    Inventor： HILLER KARL-HEINZ ,  KINDLER HUBERT ,  SCHOLZ HEINRICH ,  STROHMEYER MAX

    IPC: C07C2/68

    Abstract: 1,170,123. p-Dialkylbenzenes. BADISCHE ANILIN- & SODA-FABRIK A.G. 24 Feb., 1967 [25 Feb., 1966], No. 8902/67. Heading C5E. p-Dialkylbenzenes are prepared by reacting alkylbenzenes or benzene with olefins in the presence of aluminium chloride at a temperature above 60‹ C. for a period of less than 3 minutes. C 2 -C 12 olefins are specified. The examples describe the reaction of cumene with propylene to yield p-diisopropylbenzene in admixture with the ortho- and meta-isomers, triisopropylbenzenes and tetraisopropylbenzenes.

    Production of phenylhydrazine
    29.
    发明专利
    Production of phenylhydrazine 未知

    公开(公告)号：GB1133841A

    公开(公告)日：1968-11-20

    申请号：GB1191866

    申请日：1966-03-18

    Applicant: BASF AG

    Inventor： KINDLER HUBERT ,  SCHULER DOMINIK

    IPC: C07C241/02

    Abstract: 1,133,841. Production of phenylhydrazine. BADISCHE ANILIN- & SODA-FABRIK A.G. 18 March, 1966 [20 March, 1965], No. 11918/66. Heading C2C. Phenylhydrazine or salts thereof are obtained by the reduction of phenyl diazonium salts by means of sulphurous acid or salts thereof in aqueous medium wherein the reaction is commenced at from - 5‹ to + 50‹ C. and substantially an alkali or alkaline earth metal hydrogen sulphite (i.e. which may contain sulphurous acid or sulphite) is used as reducing agent in at least a 30 mole per cent stoichiometric excess and the reaction is completed by maintaining the reaction mixture at a higher temperature in the range of from 10‹ to 150‹ C. The sulphite solution preferably does not contain more than 25 mole per cent of free sulphurous acid or 60 mole per cent of sulphite (based on hydrogen sulphite) and the reduction is completed by maintaining the reactive mixture at 10‹ to 150‹ C., optionally with the addition of a mineral acid. The process may be effected batchwise or continuously, in the latter case the sulphur dioxide liberated during the reaction being absorbed, e.g. in caustic soda solution, and the sulphite and hydrogen sulphite solution thus formed may be recycled.

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