GB893809A - Improvements in the separation of mixtures which contain a non-volatile complex catalyst - Google Patents

Improvements in the separation of mixtures which contain a non-volatile complex catalyst

Info

Publication number
GB893809A
GB893809A GB5574/60A GB557460A GB893809A GB 893809 A GB893809 A GB 893809A GB 5574/60 A GB5574/60 A GB 5574/60A GB 557460 A GB557460 A GB 557460A GB 893809 A GB893809 A GB 893809A
Authority
GB
United Kingdom
Prior art keywords
complex
separated
stream
butyl
mixtures
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
GB5574/60A
Inventor
Hubert Kindler
Hans Georg Trieschmann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Badische Anilin and Sodafabrik AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BASF SE, Badische Anilin and Sodafabrik AG filed Critical BASF SE
Priority to DEJ17671A priority Critical patent/DE1163304B/en
Priority to FR818900A priority patent/FR1248895A/en
Publication of GB893809A publication Critical patent/GB893809A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C209/00Preparation of compounds containing amino groups bound to a carbon skeleton
    • C07C209/60Preparation of compounds containing amino groups bound to a carbon skeleton by condensation or addition reactions, e.g. Mannich reaction, addition of ammonia or amines to alkenes or to alkynes or addition of compounds containing an active hydrogen atom to Schiff's bases, quinone imines, or aziranes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Gas Separation By Absorption (AREA)

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.
GB5574/60A 1959-02-18 1960-01-20 Improvements in the separation of mixtures which contain a non-volatile complex catalyst Expired GB893809A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DEJ17671A DE1163304B (en) 1959-02-18 1960-02-10 Process for the production of hydrogen cyanide
FR818900A FR1248895A (en) 1959-02-18 1960-02-18 Improvements in the production of hydrocyanic acid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE893809X 1959-02-18

Publications (1)

Publication Number Publication Date
GB893809A true GB893809A (en) 1962-04-11

Family

ID=6846828

Family Applications (1)

Application Number Title Priority Date Filing Date
GB5574/60A Expired GB893809A (en) 1959-02-18 1960-01-20 Improvements in the separation of mixtures which contain a non-volatile complex catalyst

Country Status (1)

Country Link
GB (1) GB893809A (en)

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