Abstract:
PROBLEM TO BE SOLVED: To obtain the subject solution which does not contain a noticable amount of coloration components at all and contain a relatively low amount of hydrolyzable chlorine by directly treating them with hydrogen at a relatively low temperature and pressure without additive temperature treatment and stress. SOLUTION: A solution containing at least one kind of isocyanate is phosgenated then treated with hydrogen before the perfect removal of the solvent. The treatment with hydrogen is carried out under the pressure of 0.5×10 -2.8×10 Pa at 70-150 deg.C in the phosgenation reagent. In a preferred embodiment, at least one of the isocyanate is an isocyanate in the group of diphenylmethane diisocyanates.
Abstract:
A method for the continuous production of alkyl esters of pentenric acid by reacting butadiene-containing C4 sections with alkanols and carbon monoxide in the presence of cobalt carbonyl catalysts and heterocyclic aromatic tertiary nitrogen bases at a temperature of 100 to 160 DEG C and under a pressure of 100 to 1200 bar, characterised in that the reaction mixture is passed essentially without remixing through a treatment zone at the rate at which it is formed at a temperature of 100 to 160 DEG C under a pressure of 250 to 1200 bar and with a residence time of 10 to 60 minutes.
Abstract:
In a process for the production of methylene-di-phenylamine from aniline (A) and formaldehyde (F) in presence of a protic acid, the condensation is carried out at 80-250 deg C and the reaction mixture in the condensation stage is homogenized in a dynamic or static mixer.
Abstract:
Gegenstand der Erfindung ist ein Verfahren zur Herstellung von Mischungen aus Diphenylmethan-diisocyanaten und Polyphenyl-polymethylen-polyisocyanaten (Roh-MDI) mit einer verminderten Iodfarbzahl und einem verminderten Chlorgehalt durch Umsetzung der entsprechenden Mischungen aus Diphenylmethan-diaminen und Polyphenyl-polymethylen-polyaminen mit Phosgen in Gegenwart mindestens eines inerten organischen Lösungsmittels bei erhöhter Temperatur, wobei man nach beendeter Phosgenierung der Reaktionsmischung in Gegenwart oder Abwesenheit des Phosgens eine Mischung aus Wasser und mindestens einem ein- oder mehrwertigen Polyoxyalkylenalkohol, vorzugsweise mit einer Funktionalität von 2 bis 3, und vorteilhafterweise einer Hydroxylzahl von 20 bis 1800, in einer wirksamen Menge, die zweckmäßigerweise besteht aus mehr als 0,01 bis 0,3 Gew.-% Wasser (i) und 0,5 bis 5 Gew.-% eines Polyoxyalkylenalkohols (ii), jeweils bezogen auf das Roh-MDI-Gewicht, einverleibt, danach das überschüssige Phosgen bzw. die noch vorliegenden Phosgenreste und das inerte organische Lösungsmittel abtrennt, dem Reaktionsprodukt gegebenenfalls bis 5 Gew.-%, bezogen auf das Roh-MDI-Gewicht, mindestens eines Antioxidans auf Phenolbasis und/oder Arylphosphit hinzugefügt und die Reaktionsmischung thermisch behandelt.
Abstract:
The invention relates to a method for the production of methylenedi(phenylamine) by reacting aniline with formaldehyde in the presence of acid catalysts. The method is characterized in that aniline and optionally an acid catalyst are treated in a semi-continuos method; formaldehyde and optionally an acid catalyst are fed through a mixing organ in a circuit in which aniline, optionally an acid catalyst and optionally an already added formaldehyde are circulated and tempering the reaction mixture at a temperature of over 75 DEG C after feeding at least 50 % of the total amount of formaldehyde. The invention also relates to a method for the production of polyisocyanates by phosgenating the amines thus obtained and the polyisocyanates obtained according to this method.
Abstract:
Prodn. of mixts. of diphenylmethanedi-isocyanates and polyphenyl-polymethylene-polyisocyanates (i.e. crude MDI) with a low iodine number and a low chlorine content comprises (a) reacting the corresp. mixts. of diamines and polyamines (MDA) with phosgene in presence of inert solvent(s) at elevated temp., (b) removing excess phosgene and solvent and (c) thermal treatment of the prod.. After phosgenation (a), an effective amt. of a mixt. (I) of water and mono- or polyhydric polyoxyalkylene alcohol(s) (II) is added to the reaction mixt. in the presence or absence of phosgene.
Abstract:
In the prodn. of mixts. (crude MDI) (I) of diphenylmethane diisocyanates and polyphenyl-polymethylene polyisocyanates by reacting corresp. mixts. of diphenylmethane diamines and polyphenyl-polymethylene polyamines with COCl2 in the presence of inert organic solvent(s) (II) at elevated temp., the I2 colour no. is reduced by adding phenols (III) after phosgenation and before sepg. excess COCl2 and (II) and heat treatment of the reaction prod.Pref. (III) may be mono- or polyhydric and pref. polycyclic. They are added in amts. of 0.001-10 (wt.%) w.r.t. (I) in the reaction mixt., pref. when the mixt. contains 0.01-3% COCl2.
Abstract:
Prodn. of butanedicarboxylic acid methyl esters (I) is effected by reacting a methyl pentenoate (II) with CO and MeOH in the presence of pyridine and/or picolines (III) and a Co catalyst at elevated temp. and pressure, and treating the reaction mixt. with an O2-contg. gas and aq. HOAc. (III) are recovered by (a) sepg. the reaction mixt. into an aq. phase contg. Co(OAc)2, (III), HOAc and MeOH, and an organic phase contg. (I), by-products, (II), HOAc and (III); (b) extracting (III) from the organic phase with aq. HOAc; (c) combining the extract with the aq. phase; and (d) distilling (III) from the mixt. to leave an aq. soln. contg. Co(OAc)2 and HOAc.
Abstract:
The production of methylene-di-phenylamine from aniline (A) and formaldehyde (F) with an acid catalyst (C) comprises placing (A) and possibly (C) in a reactor, feeding (F) and possibly (C) through a mixer into a circulation loop containing (A), possibly (C) and possibly (F), and heating to above 75 degrees C after adding at least 50% of the total (F). Independent claims are also included for: (a) mixtures containing methylene-di-phenylamine (MDA) obtained by this process; (b) a process for the production of polyisocyanates by phosgenation of these mixtures; (c) a process for the production of methylene-diphenylisocyanate (MDI) by phosgenation of MDA (obtained as above) at 50-150 degrees C and 0.5-10 bar, optionally in presence of inert solvent; (d) a process for the production of MDI comprising: (1) the semi-continuous process described above using a mol ratio of (A):(C) = (1:0.6)-(1:0.01) and a mol ratio of (A):(total F) = (1.7:1)-(7.2:1), in which the temperature of the circulating mixture is 20-75 degrees C and the mixture is heated for at least 0.2 hour at above 75 degrees C after adding at least 50% of the (F), (2) neutralization, (3) distillation of water and aniline, (4) phosgenation of the purified MDA as in (c) above, (5) removal of phosgene, hydrogen chloride and possibly solvent at below 150 degrees C under vacuum or inert gas, (6) removal of solvent at not above 1900 degrees C and (7) isolation of 2,2'-, 2,4'- and/or 4,4'-MDI and/or mixtures of at least two of these isomers by distillation at 2-50 mbar and 150-250 degrees C and/or by crystallization; and (e) polyisocyanates obtained by these processes.
Abstract:
Solutions containing at least an isocyanate (I) are prepared by treatment with hydrogen, without the formation of an over pressure after the phosgenation step and prior to separation of the solvent.