Abstract:
The invention relates to a method for hydrogenating aliphatic alpha-, omega-dinitriles in the presence of a heterogeneous fixed-bed catalyst. The method is characterised in that the reaction mixture contains 2 mu mol to 30 mmol Na, K, Rb, Cs, Mg, Ca, Sr, Ba or Mn or mixtures thereof in the form of a basic salt, in relation to 10 mol of the aliphatic alpha-, omega-dinitrile used.
Abstract:
The invention concerns a process for simultaneously preparing 6-aminocapronitrile and hexamethylene diamine proceeding from a mixture which contains a phosphorated compound and substantially adipodinitrile and is obtained by reacting butadiene with hydrocyanic acid in the presence of a catalyst containing a phosphorated compound. The process is characterized in that: (1) the portion by weight of a phosphorated compound, calculated as phosphorus, in the mixture is reduced; (2) the resultant mixture is partially hydrogenated in the presence of a catalyst in order to form an alpha-, omega aminonitrile; and (3) 6-aminocapronitrile and hexamethylene diamine are separated from the mixture.
Abstract:
Herstellung von NH2-Gruppen enthaltenden Verbindungen durch Hydrierung von Verbindungen, die mindestens eine ungesättigte Kohlenstoff-Stickstoff-Bindung enthalten, mit Wasserstoff in Gegenwart eines Katalysators bei Temperaturen von nicht unterhalb Raumtemperatur und erhöhtem Wasserstoff-Partialdruck gewünschtenfalls in Gegenwart eines Lösungsmittels, indem man (a) als Katalysator einen Cobalt- und/oder Eisen-haltigen Katalysator einsetzt, und (b) nach Absinken des Umsatzes, bezogen auf die zu hydrierende Verbindung, und/oder der Selektivität, bezogen auf das gewünschte Produkt, unter einen definierten Wert oder nach Ansteigen der Menge eines unerwünschten Nebenproduktes über einen definierten Wert, die Hydrierung unterbricht, indem man die Zufuhr der zu hydrierenden Verbindungen sowie gewünschtenfalls vorhandenem Lösungsmittel stoppt, (c) den Katalysator bei einer Temperatur im Bereich von 150 bis 400 DEG C mit Wasserstoff behandelt, wobei man dem Wasserstoffdruck im Bereich von 0,1 bis 30 MPa und die Behandlungszeit im Bereich von 2 bis 48 h wählt, und (d) anschliessend die Hydrierung der mindestens eine ungesättigte Kohlenstoff-Stickstoff-Bindung enthaltenden Verbindungen fortsetzt, sowie Regenerierung von Cobalt- und/oder Eisen-haltigen Katalysatoren.
Abstract:
The invention concerns catalysts suitable for preparing aliphatic alpha-, omega-aminonitriles by partial hydrogenation of aliphatic dinitriles, containing: (a) metallic cobalt, a cobalt compound or their mixtures, the metallic cobalt portion being between 20 and 100 wt % relative to (a); (b) between 10 and 70 wt %, relative to (a), of metallic iron, iron oxide, a further iron compound or their mixtures, the iron oxide portion being between 20 and 100 wt % relative to (b); and (c) between 0 and 1 wt %, relative to (a), of a compound based on an alkali metal, alkaline earth metal or zinc.
Abstract:
Process for the separation of 2-aminomethylcyclopentylamine from a mixture containing hexamethyldiamine and 2-aminomethylcyclopentylamine, characterized by the fact that the separation is carried out by means of distillation at a pressure of 1-300 mbars.
Abstract:
A process for producing 2-cyano-3,3-diary acrylic acid esters of general formula (I) in which R and R are hydrogen, C1-C12 alkoxy groups or di-(C1-C4 alkyl) amino groups and R is a C4-C18 alkyl group which may be interrupted by oxygen atoms in the ether function, by the reaction of benzophenonimine of general formula (II) with a cyanic acid ester of general formula (III), in which the reaction is conducted at 20 to 60 DEG C and the ammonia released is continuously removed from the reaction mixture with the aid of a stream of gas or by reducing the pressure to 900 to 100mbar.
Abstract:
Described are 2-cyanoacrylic acid esters (I) in which the groups are defined as follows: R and R are hydrogen or a group with an isocyclic or heterocyclic ring system having at least one iso-aromatic or hetero-aromatic nucleus, whereby one of the groups R and R must be different from hydrogen, n is from 2 to 10, X in the case when n = 2 is a group of the formula (II) in which m is from 2 to 8, X in the case when n > 2 is an n-hydric aliphatic or cycloaliphatic polyol group with 3 to 20 C-atoms, whereby the cycloaliphatic polyol group may include 1 to 2 hetero-atoms and the aliphatic polyol group may include up to 8 non-adjacent oxygen atoms, sulphur atoms, imino groups or C1-C4 alkylimino groups in the carbon chain. Compounds of the formula (I) are suitable for use as light-protection agents.
Abstract:
A method for catalytic hydrogenation of adipodinitrile into hexamethylene diamine at a high temperature and high pressure in the presence of catalysts based on elementary iron as a catalytically active constituent and ammonia as a solvent. The invention is characterized in that a) adipodinitrile is hydrogenated at temperatures ranging from 70 to 220 °C and at pressures of 100-400 bars in the presence of catalysts based on elementary iron and ammonia as a solvent to obtain a mixture containing adipodinitrile, 6-aminocapronitrile, hexamethylene diamine and high boilers until the sum of the 6-aminocapronitrile and adipodinitrile concentrations amount to 1-50 wt. % in relation to the ammonia-free hydrogenation mixture; b) ammonia is separated from the hydrogenation product; c) hexamethylene diamine is separated from the remaining mixture; d) 6-aminocapronitrile and adipodinitrile are separated individually or jointly from high boilers and e) 6-aminocapronitrile, adipodinitrile or the mixtures thereof are returned to step a).
Abstract:
The invention relates to a method for producing polymethylol compounds of formula (I), in which R represents a further methylol group or an alkyl group with between 1 and 22 C atoms or an aryl or alkyl aryl group with between 6 and 22 C atoms, by condensating aldehydes with between 2 and 24 C atoms with formaldehyde, using tertiary amines as catalysts, with a view to obtaining compounds of formula (II), in which R has the meaning assigned to it above. The invention further relates to a process for hydrogenating polymethylol compounds by condensation in stages. For this, a) in a first (reaction) stage, the aldehydes with 2 or more C atoms are reacted with 2 to 8 times the molar quantity of formaldehyde in the presence of a tertiary amine as catalyst; b) in a second (separation) stage, either the reaction mixture is separated into a distillation residue containing primarily the compounds of formula (II) and a destillation flow containing primarily the compounds of unreacted or partly reacted starting materials which is fed back to the first stage, or the reaction mixture of the first stage is separated into an aqueous and an organic phase by means of a phase separation device and the organic phase fed back to the first stage, and c) in a third (post-reaction distillation) stage, the distillation residue of the second stage or the aqueous phase obtained by phase separation during the second stage is subjected to a catalytic and/or heat treatment, the compound of formula (III) which has not been fully methylolized is transformed into the corresponding compound of formula (II) and into the corresponding methylene compound of formula (IV), in which R' represents hydrogen or has the meaning assigned above to R, the reaction mixture obtained in this way is distilled, and the distillation overhead product, which contains a compound of formula (IV) and unreacted formaldehyde, is fed back to the first stage. Thereafter, the still bottom of this distillation process, which essentially contains the compound of formula (II), is hydrogenated in the known manner so as to obtain the corresponding end product of formula (I).