Abstract:
Die vorliegende Erfindung betrifft ein Verfahren zur Gewinnung von Rein-Anilin durch katalytische Hydrierung von Nitrobenzol und Aufarbeitung des hierbei erhaltenen Reaktionsgemisches, die die Verfahrensschritte umfasst: -katalytische Hydrierung von Nitrobenzol, -optional partielle Kondensation des Reaktionsgemisches der katalytischen Hydrierungin einer oder mehreren Stufen, -Auftrennung des nach der katalytischen Hydrierung oder der optional durchgeführten Kondensation erhaltenen Reaktionsgemisches in eine Wasserstoff enthaltende Gasphase und eine Flüssigphase und -Flüssig/Flüssig-Phasentrennung derhierbei erhaltenen Flüssigphase, unter Erhalt einer wässrigen Phase, die einer weiteren Aufarbeitung zugeführt oder ausgeschleust wird, sowie von Roh-Anilin als organische Phase, wobei das Roh- Anilin 90-95 Gew.-%Anilin, 4-9 Gew.-% Wasser und Rest Schwersieder gegenüber Anilin, jeweils bezogen auf das Gesamtgewicht des Roh-Anilins, enthält, und wobei die Summe der Komponenten des Roh-Anilins 100 Gew.-% beträgt, -destillative Vorreinigung des Roh-Anilins durch teilweise oder vollständige Abtrennung des Wassers über den Kopfstrom einer ersten Destillationskolonne unter Erhalt eines Sumpfstromes, der als Feed-Strom -einer Reinkolonne zugeführt wird, aus der über Kopf ein Rein-Anilin-Strom, enthaltend mindesten 99,9 Gew.-% Anilin, bezogen auf das Gesamtgewicht des Rein-Anilin-Stromes, sowie ein Sumpfstrom, enthaltend Schwersieder und der einer Verbrennung zugeführt wird, abgezogen werden, das dadurch gekennzeichnet ist, dass der Gewichtsanteil des Sumpfstromes ausder Reinkolonne auf maximal 0,8 %, bezogen auf das Gewicht des Feed-Stromes begrenzt wird, und dadurch gewährleistet wird, dass derselbe unter entsprechender Begleitbeheizung der hierfür vorgesehenen Leitungen, die gewährleistet, dass die Temperatur des darin geförderten Stromes 45°C oder höher ist, pumpfähig ist, indem dem Sumpfstrom Methanol, Ethanol, Propanol, Aceton oder Mischungen hiervon in einem Gewichtsanteil von 5-30%, bezogen auf das Gewicht des Sumpfstromes, zugesetzt wird.
Abstract:
The invention provides a process for simultaneously preparing 4,4'-diphenylmethanediamine and diphenylmethane diisocyanate and polyphenylenepolymethylene polyisocyanates, comprising the steps of a) preparing a mixture of diphenylmethanediamine and polyphenylenepolymethylenepolyamines by acidic condensation of aniline and formaldehyde and subsequent workup of the mixture, b) removing a portion of the mixture prepared in step a), c) distilling the mixture removed in step b) in a column, d) recycling the bottom product from step c) to the end product from step a) and condensing the top product from step c), e) distilling the top product from step c) in a column, f) recycling the top product from step e) to the end product from step a), g) recovering the 4,4'-diphenylmethanediamine obtained as the bottom product in step e), h) reacting the mixture from step a) with phosgene and subsequently working up the reaction product.
Abstract:
In a process for extracting (chlorinated) hyrocarbon-free hydrogen chloride and phosgene-free (chlorinated) hydrocarbons from a hydrogen chloride stream containing (chlorinated) hydrocarbons and phosgene, (i) the fresh hydrogen chloride stream containing phosgene and (chlorinated) hydrocarbons is led in a first step first through a first adsorber and then through a second adsorber interconnected in series, until essentially no more (chlorinated) hydrocarbon is adsorbed by the first adsorber; (ii) the fresh hydrogen chloride stream is led in a second step through the second adsorber, while the first adsorber is regenerated, substantially phosgene-free (chlorinated) hydrocarbon being produced during regeneration; (iii) the fresh hydrogen chloride stream is led in a third step first through the second adsorber and then through the regenerated first adsorber, until substantially no more (chlorinated) hydrocarbon is adsorbed by the second adsorber; (iv) the fresh hydrogen chloride stream is led in a fourth step through the first adsorber, while the second adsorber is regenerated, a substantially phosgene-free (chlorinated) hydrocarbon being produced during regeneration, and steps (i) to (iv) can be successively repeated one or more times.
Abstract:
The invention relates to a method for producing isocyanates by reacting amines with phosgene in the presence of inert organic solvents inside a reactor and by subsequently processing the reaction mixture exiting the reactor. The invention is characterized in that the separating out of the solvent ensues in a two-step or multi-step, preferably two-step distillation process, and the solvent is separated out in a first apparatus under a pressure of 0.1 to 15 bar and in a second or other apparatuses under a pressure of 1 to 900 mbar. The condensation heat of the solvent vapor from the first apparatus is used for partially or completely vaporizing solvent in the second apparatus.
Abstract:
The invention relates to a method for obtaining pure aniline by catalytically hydrogenating nitrobenzene and reprocessing the reaction mixture obtained therefrom, having the following method steps: - the catalytic hydrogenation of nitrobenzene; - optionally the partial condensation of the reaction mixture of the catalytic hydrogenation in one or more stages; - the separation of the reaction mixture obtained after the catalytic hydrogenation or the condensation, which is optionally carried out, into a gas phase, which contains hydrogen, and a liquid phase; - the liquid-liquid phase separation of the liquid phase obtained in the separation step, thereby obtaining an aqueous phase, which is further reprocessed or discharged, and raw analine as an organic phase, said raw analine containing 90-95 wt.% aniline, 4-9 wt.% water, and residual high boilers relative to the analine, in each case based on the total weight of the raw analine, and the sum of the components of the raw analine equaling 100 wt.%; and - the pre-cleaning of the raw analine by partly or completely separating the water via the head stream of a first distillation column, thereby obtaining a bottom stream that is fed as a feed stream to a purification column from which a pure aniline stream containing at least 99.9 wt.% aniline based on the total weight of the pure analine stream is drawn via the head and a bottom stream containing high boilers is drawn and fed to a combustion process. The invention is characterized in that the weight ratio of the bottom stream from the purification column is limited to maximally 0.8% relative to the weight of the feed stream, thereby ensuring that said bottom stream can be pumped under the effect of a corresponding trace heating of the lines provided for this purpose, said trace heating ensuring that the temperature of the stream conducted in the lines is 45 °C or higher, wherein the bottom stream is exposed to methanol, ethanol, propanol, acetone, or mixtures thereof in a weight ratio of 5-30% based on the weight of the bottom stream.