摘要:
Cobalt catalysts whose catalytically active composition comprises from 55 to 98% by weight of cobalt, from 0.2 to 15% by weight of phosphorus, from 0.2 to 15% by weight of manganese and from 0.05 to 5% by weight of alkali metal, calculated as oxide, are prepared by calcining the catalyst composition, reducing it at final temperatures of from 200.degree. to 400.degree. C. in a stream of hydrogen and subsequently surface-oxidizing it by treatment in a stream of air at final temperatures of from 20.degree. to 60.degree. C. and can be used in a process for hydrogenating organic nitriles and/or imines.
摘要:
Process for the preparation of diamines of the general formula I ##STR1## in which A denotes a C.sub.1 -C.sub.20 alkylene chain optionally mono- to penta-substituted by C.sub.1 -C.sub.4 alkyl,R.sup.1, R.sup.2 denote C.sub.1 -C.sub.20 alkyl, C.sub.1 -C.sub.20 hydroxyalkyl, C.sub.3 -C.sub.8 cycloalkyl, C.sub.4 -C.sub.20 alkylcycloalkyl, C.sub.4 -C.sub.20 cycloalkylalkyl, phenyl, C.sub.7 -C.sub.20 phenylalkyl, C.sub.1 -C.sub.20 alkoxyalkyl, C.sub.7 -C.sub.20 phenoxyalkyl or together a saturated or unsaturated C.sub.2 -C.sub.6 alkylene chain optionally monosubstituted, disubstituted, or trisubstituted by C.sub.1 -C.sub.4 alkyl and optionally interrupted by oxygen or nitrogen,by the reaction of dinitriles of the general formula IINC--A--CN (II),in which A has the aforementioned meaning,with secondary amines of the general formula II ##STR2## in which R.sup.1 and R.sup.2 have the aforementioned meanings, with hydrogen at temperatures ranging from 50.degree. to 200.degree. C. and pressures ranging from 5 to 300 bar in the presence of a hydrogenation catalyst, in which a palladium catalyst on an oxidic support is used as hydrogenation catalyst.
摘要:
A process for the purification of tertiary amines in a crude mixture contaminated with undesirable primary and secondary amines which may have only a slight variance in boiling point with respect to the tertiary amine, wherein the crude mixture of the tertiary amine is treated at temperatures which may range from 0.degree. to 200.degree. C. but preferably from 20 to 150.degree. C. and at pressures of from 1 to 200 bar but most preferably under atmospheric pressure with a carboxylate of the formula ##STR1## in which R.sup.4 and R.sup.5 are selected from the group consisting of C.sub.1 -C.sub.20 -alkyl, C.sub.3 -C.sub.12 -cycloalkyl, C.sub.4 -C.sub.20 -cycloalkylalkyl, and aryl or C.sub.7 -C.sub.20 -aralkyl, both optionally mono- to penta- substituted by C.sub.1 -C.sub.8 -alkyl, C.sub.3 -C.sub.8 -cycloalkyl, or C.sub.4 -C.sub.12 -cycloalkylalkyl, and R.sup.4 may also represent hydrogen,to selectively form the alkylamides of the primary and secondary amine contaminants; and then separating the alkylamides from the tertiary amine by distillation.
摘要:
A process for the preparation of polyalcohols comprises the stages:(a) Reaction of an alkanal or ketone with formaldehyde in aqueous solution in the presence of a tertiary amine, to form a formates containing polyalcohol product mixture,(b) removal of water, excess tertiary amine, excess formaldehyde(c) heating of remaining mixture from (b) with removal of further formaldehyde and tertiary amine with formation of the formates of the polyalcohol,(d) transfer of tertiary amine removed from stage (b) and/or from stage (c), to synthesis stage (a) and/or to the subsequent transesterification stage (e),(e) transesterification of the resulting formates of the polyalcohol from stage (c) with an alcohol of the formula ROH in the presence of a transesterification catalyst to give polyalcohols and formates of the formula ##STR1## where R is a hydrocarbon radical, preferably alkyl of 1-6, particularly preferably 1-2, carbon atoms, and(f) isolation of the polyalcohols.
摘要:
The invention relates to a process for reducing the dimerization of piperidines of the formula I ##STR1## where R.sup.1 to R.sup.4 are C.sub.1 - to C.sub.6 -alkyl, R.sup.1 and R.sup.2 and/or R.sup.3 and R.sup.4 together are a CH.sub.2 chain having 2 to 5 carbon atoms, which comprises adding to the piperidine from 0.001 to 0.2% by weight of a reducing agent of the formula MXH.sub.4-m Y.sub.m, where M is an alkali metal, NR.sub.4, where R are identical or different C.sub.1 -C.sub.4 -alkyl groups, or an equivalent of an alkaline earth metal or an equivalent of zinc, X is boron or aluminum, Y is H or CN and m is 0 or 1. The invention also relates to a mixture of piperidines of the formula I, from 0.001 to 0.2% by weight of a reducing agent and from 1 to 1000 ppm of dimers of the piperidines of the formula I, and to the preparation of hindered amine light stabilizers therefrom.
摘要:
A process for preparing N-methyl-2-(3,4-dimethoxyphenyl)-ethylamine comprises hydrogenating 3,4-dimethoxyphenylacetonitrile with a methylamine of the general formula I ##STR1## where R.sup.1 is hydrogen, benzyl or tert-butyl, and hydrogen in the presence of a supported catalyst which comprises from 0.05 to 50% by weight of copper chromite, copper, silver, gold, iron, cobalt, nickel, ruthenium, rhodium, palladium, osmium, iridium, platinum or mixtures thereof, in the presence or absence of water at from 20.degree. to 200.degree. C. under from 1 to 300 bar.
摘要:
Caprolactam and hexamethylenediamine are prepared simultaneously starting from adiponitrile by a process in which (a) adiponitrile is partially hydrogenated to give a mixture containing essentially 6-aminocapronitrile, hexamethylenediamine, ammonia, adiponitrile and hexamethyleneimine, (b) the mixture obtained in (a) is subjected to a distillation to give ammonia as the top product and a bottom product I, (c) the bottom product I containing essentially 6-aminocapronitrile, hexamethylenediamine, adiponitrile, hexamethyleneimine, inert compound A and ammonia, the ammonia content being lower than that of the mixture used in stage (b), is subjected to a second distillation to give a mixture comprising the inert compound A and ammonia as the top product and a bottom product II, (d) the bottom product II is subjected, in a third column, to a distillation to give the inert compound A as the top product and a bottom product III, (e) the bottom product III is subjected, in a fourth column, to a distillation to give a top product KP1, containing essentially hexamethyleneimine and a bottom product IV, (f) the top product KP1 is subjected, in a fifth column, to a distillation to give a top product KP2, which contains essentially hexamethyleneimine, and (g) the bottom product IV containing essentially 6-aminocapronitrile and adiponitrile is subjected, in a sixth column, to a distillation to give 6-aminocapronitrile, and the 6-aminocapronitrile thus obtained is then cyclized to give caprolactam.
摘要:
3-Aminomethyl-3,5,5-trimethylcyclohexylamine is prepared by reacting 3-cyano-3,5,5-trimethylcyclohexanone with 3-aminomethyl-3,5,5-trimethylcyclohexylamine and subsequently or simultaneously adding ammonia under a hydrogen pressure of from 50 to 300 bar in the presence of a hydrogenation catalyst at from 20.degree. to 150.degree. C., by a process in which the reaction is carried out without removing the water of reaction.
摘要:
Aliphatic alpha, omega-aminonitriles are prepared by partial hydrogenation of aliphatic alpha, omega-dinitriles at elevated temperatures and superatmospheric pressure in the presence of a solvent and of a catalyst by a process which comprises using a catalyst which(a) contains a compound based on a metal selected from the group consisting of nickel, cobalt, iron, ruthenium and rhodium and(b) contains from 0.01 to 25% by weight, based on (a), of a promoter based on a metal selected from the group consisting of palladium, platinum, iridium, osmium, copper, silver, gold, chromium, molybdenum, tungsten, manganese, rhenium, zinc, cadmium, lead, aluminum, tin, phosphorus, arsenic, antimony, bismuth and rare earth metals and(c) from 0 to 5% by weight, based on (a), of a compound based on an alkali metal or on an alkaline earth metal,with the proviso that the component (a) is not based on iron or iron and one of the metals selected from the group consisting of cobalt, ruthenium and rhodium when (b) is a promoter based on a metal selected from the group consisting of titanium, manganese, chromium and molybdenum, and with the further proviso that, when a compound based on only ruthenium or rhodium or ruthenium and rhodium or nickel and rhodium is selected as component (a), the promoter (b) may be dispensed with.
摘要:
In a process for preparing a bicyclic amidine by reacting a lactone and a diamine with elimination of water, water formed by elimination is removed from the reaction mixture during the reaction. A diazabicycloalkene, a process for its preparation and its use are also described.