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    • 6. 发明公开
    • VERFAHREN ZUR REINIGUNG VON CAPROLACTAM
    • 程序对清洁己内酰胺
    • EP1565435A1
    • 2005-08-24
    • EP03789024.1
    • 2003-11-11
    • BASF Aktiengesellschaft
    • LUYKEN, HermannANSMANN, AndreasBENISCH, ChristophBASSLER, PeterFISCHER, Rolf-HartmuthMAIXNER, StefanMELDER, Johann-Peter
    • C07D201/16C07D201/08
    • C07D201/16
    • The invention relates to a method for purifying crude caprolactam that has been obtained by: 1) reacting a mixture (I) containing 6-aminocapronitrile and water to form a mixture (II) containing caprolactam, ammonia, water, high boilers and low boilers in the presence of a catalyst followed by; 2) removing ammonia from mixture (II) while obtaining a mixture (III) that contains caprolactam, water, high boilers and low boilers, after which; 3) water is entirely or partially removed from mixture (III) while obtaining a crude caprolactam (IV) that contains caprolactam, high boilers and low boilers. The inventive method is characterized in that: a) the crude caprolactam and an inorganic acid, which has a boiling point higher that that of caprolactam under distillation conditions in accordance with subsequent steps b) to h), are fed to a first distillation device K1; b) the crude caprolactam and the inorganic acid are distilled in the first distillation device K1 during which a first partial flow in the bottom area and a second partial flow in the top area are withdrawn from the distillation device K1; c) the second partial flow from step b) is fed to a second distillation device K2; d) the second partial flow from step b) is distilled in the second distillation device K2 during which a first partial flow in the bottom area and a second partial flow in the top area are withdrawn from the distillation device K2; e) a first partial flow from step d) is fed to a third distillation device K3; f) the first partial flow from step d) is distilled in the third distillation device K3 during which a first partial flow in the bottom area and purified caprolactam in the top area are withdrawn from the distillation device K3, and; g) the first partial flow from step f) is fed to the first distillation device K1.
    • 7. 发明授权
    • VERFAHREN ZUR ABTRENNUNG VON AMMONIAK
    • 用于分离氨
    • EP1299347B1
    • 2005-04-27
    • EP01957948.1
    • 2001-07-10
    • BASF AKTIENGESELLSCHAFT
    • LUYKEN, Hermann
    • C07C231/24C07D201/16
    • C07C231/24C07D201/16
    • The invention relates to a method for separating ammoniac (I) from mixtures (II) containing ammoniac (I) and an amide (IV) is obtained by reacting educts (III) selected from the group consisting of nitriles (IIIa), amines (IIIb), aminonitriles (IIIc) and aminoamides (IIId) with water. The method is characterised in that a) the educt (III) is reacted with water in liquid phase in the presence of an organic liquid diluting agent (V) to form a mixture (II) containing amide (IV) and ammoniac (I), b) the mixture (II) is transformed under conditions of mass, pressure and temperature - under which the diluting agent (V) and the water are in a liquid state and exhibit a miscibility gap - in order to obtain a two phase system consisting of a phase (VII), c) phase (VII) is separated from phase (VIII), d) the ammoniac present in phase (VII) is separated by extraction (a) by means of a mixture (IX) containing water in order to obtain a mixture (XI) which contains less ammoniac than phase (VII), and e) the diluting agent (V) is separated from the mixture (XI) in order to obtain the amide (IV).