摘要:
A process is disclosed for the purification, by distillation, of trimethylolpropane originating from the hydrogenation of 2,2-dimethylolbutanal, said process including the following steps: (a) reaction of n-butyraldehyde with formaldehyde in the presence of catalytic amounts of a tertiary amine, and hydrogenation of the resulting mixture to give a mixture containing trimethylolpropane; (b) separation of water, methanol, trialkylamine and/or trialkylammonium formate by distillation; (c) heating of the residue obtained in (b) under reduced pressure to a temperature at which TMP is volatile and compounds boiling above TMP are cleaved, in order to separate off, by distillation, TMP and compounds more volatile than TMP; (d) distillation of the distillate obtained in (c) in order to separate off the more volatile compounds and recover pure TMP; and (e) optional distillation of the TMP obtained in (d) in order to recover TMP with a low APHA color index. A process is also disclosed in which trialkylammonium formate is distilled under mild conditions from crude mixtures of polyhydric alcohols, predominantly trimethylolpropane.
摘要:
Formaldehyde is removed by distillation from reaction solutions containing a methlolated alkanal which was obtained from the reaction of formaldehyde with an alkanal which has at least one acidic hydrogen atom &agr; to the carbonyl function or from the reaction of a 2-alkylacrolein or acrolein with water and formaldehyde, by a process in which this reaction was carried out in the presence of catalytic amounts of organic amine. The process permits the improved removal of formaldehyde from the reaction mixture and furthermore facilitates the hydrogenation of the alkanals thus obtained to give polyols.
摘要:
A process for greatly improving the color index of polyhydric alcohols, especially trimethylolpropane, by hydrogenation comprises using, in the hydrogenation, an alcohol which has already been purified by distillation. The catalysts used are those conventionally employed in hydrogenations, preferably copper, nickel, palladium or ruthenium catalysts.
摘要:
A process is provided for increasing the yield in the preparation of polyhydric alcohols obtained from methylolated alkanals by hydrogenation, wherein derivatives of these alcohols are decomposed by adding 5 ppm to 1% by weight, preferably 100 to 1000 ppm, of a suitable acid to an anhydrous mixture containing these derivatives, heating the mixture to temperatures of 100 to 300° C. and then separating off the polyhydric alcohol by distillation. This process makes it possible simply and efficiently to decompose compounds which boil above the polyhydric alcohol and are unwanted by-products of its synthesis.
摘要:
Methylolalkanal of the formula II (R=CH2OH, C1-C22-alkyl, aryl or C6-C22-aralkyl) is prepared spe-wise by a) reacting a C2-C24-aldehyde with formaldehyde in the presence of a tertiary amine, b) separating the reaction mixture i) into a bottom fraction comprising the compound of formula II and an incompletely methylolated compound of the formula III and a distillate stream comprising unconverted or partially converted starting materials, or ii) into an aqueous phase and an organic phase, and recycling the distillate stream or the organic phase to a), and c) subjecting the bottom fraction or the aqueous phase i) to a catalytic or thermal reaction to convert the compound of formula III to the compound of formula II and to a corresponding methylene compound of formula IV (R′=H or R) and ii) separating the reaction product into an overhead stream comprising the compound of formula IV and unconverted formaldehyde which is recycled to a), and a bottom fraction comprising the compound of formula II.
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:
Process for producing polyamides that are stable during processing, by treating the polyamide during the solid-phase postcondensation process with a gas which comprises carrier gas (inert gas), water, and acid, or an anhydride or lactone or a mixture of these or, respectively, comprises ammonia, or amine, or a mixture of these, at a temperature from 130 to 200° C. and at a pressure of from 0.01 to 10 bar.
摘要:
A process for preparing water-absorbing polymer beads by polymerizing droplets of a monomer solution in a gas phase surrounding the droplets, the initiator being added to the monomer solution from 0.5 to 60 seconds before the droplets are generated.
摘要:
A process for removing trioxane from a mixture I of formaldehyde, trioxane and water, by a) distilling the mixture I in a first distillation stage at a pressure of from 0.1 to 2 bar to obtain a stream II which comprises formaldehyde and a stream III which comprises predominantly trioxane and additionally water and formaldehyde, b) mixing the stream III with a recycle stream VII which comprises predominantly trioxane and additionally water and formaldehyde to obtain a stream IIIa which comprises predominantly trioxane and additionally water and formaldehyde, c) distilling the stream IIIa, if appropriate after removing low boilers from the stream III or IIIa in a further distillation stage, in a second distillation stage at a pressure of from 0.2 to 10 bar, the pressure in the second distillation stage being at least 0.1 bar higher than the pressure in the first distillation stage, to obtain a stream IV of trioxane and a stream V which comprises predominantly trioxane and additionally water and formaldehyde, d) distilling the stream V in a third distillation stage at a pressure of from 0.1 to 4 bar to obtain a stream VI which comprises predominantly water and additionally formaldehyde, and the recycle stream VII which comprises predominantly trioxane and additionally water and formaldehyde, e) if appropriate, distilling the stream VI in a fourth distillation stage to obtain a stream VIII which comprises predominantly water, and a stream IX which comprises predominantly formaldehyde.
摘要:
The present invention relates to a process for producing moldings comprising (A) at least one lactam, (B) at least one activator, and (C) at least one catalyst, where (A) to (C) proceed through treatments comprising a) mixing of (A), (B), and (C), b) metering of (A), (B), and (C) into an apparatus for producing mixture droplets, and producing mixture droplets, and c) depositing the mixture droplets comprising (A), (B), and (C) on a belt, and d) producing moldings.