Abstract:
In a dividing wall column comprising as segments a) an upper column region (6), b) an inflow section (7), c) an offtake section (8) and d) a lower column region (9), the inflow section b) (7) and the offtake section c) (8) are separated from one another laterally by a dividing wall (10) fixed in the column and the dividing wall (10) is located between the upper column region a) (6) and the lower column region d) (9). The present invention provides for the dividing wall (10) to be constructed at least partly of an elastic material, the dividing wall (10) to have a slightly overdimensional width and the dividing wall (10) to be fixed in the column by the dividing wall exercising an elastic recovery force on the interior wall of the column. The dividing wall can easily be installed in, in particular, relatively small columns.
Abstract:
A process for preparing at least one unsaturated alcohol (B) comprises the steps (I) to (III) below: (I) reaction of at least one alkali metal hydroxide or alkaline earth metal hydroxide with at least one alcohol (A) in at least one organic solvent (L) to give a mixture (G-I) comprising at least the alcohol (A), the solvent (L) and an alkoxide (AL); (II) reaction of at least one carbonyl compound of the formula R—CO—R′ with at least one alkyne of the formula R″—C≡C—H and the mixture (G-I) obtained in step (I) to give a mixture (G-II) comprising at least the alcohol (A), the solvent (L) and an unsaturated alcohol (B); (III) distillation of the mixture (G-II) obtained in step (II) to give the alcohol or alcohols (B) and a mixture (G-III) comprising the solvent (L) and the alcohol (A), wherein the solvent (L) obtained in step (III) and the alcohol (A) obtained in step (III) are recycled as a mixture to step (I).
Abstract:
A process for working up by distillation the crude products obtained in the process according to DE-A 196 07 954 and containing 1,6-hexanediol (HDO), 1,5-pentanediol (PDO) or caprolactone (CLO) in order to obtain the corresponding pure products, the working-up by distillation being carried out in each case in a dividing wall column (TK) in which a dividing wall (T) is arranged in the longitudinal direction of the column with formation of an upper common column region (1), a lower common column region (6), a feed section (2, 4) having a rectification section (2) and stripping section (4), and a take-off section (3, 5) having a stripping section (3) and rectification section (5), with feeding of the respective crude product HDO, PLO or CLO in the middle region of the feed section (2, 4) and removal of the high boiler fraction (C) from the bottom of the column, of the low boiler fraction (A) via the top of the column and of the medium boiler fraction (B) from the middle region of the take-off section (3, 5), or in thermally coupled columns.
Abstract:
A method of devulcanizing crosslinked rubber uses a planetary roller extruder with a central spindle, planetary spindles, a housing, and a feed part. The method includes feeding vulcanized rubber through the feed part into the housing, rotating the central spindle about its rotational axis and thereby causing the planetary spindles to rotate about their rotational axes and revolve about the central spindle. This generates mechanical and thermal stress on the vulcanized rubber by kneading and/or crushing of the vulcanized rubber, breaking or destroying the molecular chains or bonds of the vulcanized rubber. The method further includes at least one of (A) adding particles of the vulcanized rubber eccentrically to the center of the planetary roller extruder module between the planetary spindles and (B) mechanically pressing particles of the vulcanized rubber between the planetary spindles with a crammer feeder.
Abstract:
The present invention relates to a process for purifying a composition (I) at least comprising cyclododecanone. The process according to the invention for purifying a composition (I) at least comprising cyclododecanone comprises at least step (i) (i) irradiation of the composition (I).
Abstract:
The present invention relates to a process for continuously preparing 5-alkoxy-substituted oxazoles, in particular for continuously preparing 4-methyl-5-alkoxy-substituted oxazoles and also a process for preparing pyridoxine derivatives.
Abstract:
A process for preparing 1,6-hexanediol from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol after water extraction of the reaction mixture followed by extraction with aqueous sodium hydroxide solution, by esterification of the acids and hydrogenation comprises a) liberating the carboxylic acids from the alkaline extract by addition of a mineral acid, b) fractionating the organic phase comprising carboxylic acids to give a distillate comprising the low molecular weight monocarboxylic acids and a residue comprising adipic acid and 6-hydroxycaproic acid, c) reacting the monocarboxylic an dicarboxylic acids present in the aqueous dicarboxylic acid mixture with a low molecular weight alcohol to give the corresponding carboxylic esters, d) freeing the esterification mixture obtained of excess alcohol and low boilers in a first distillation step, e) fractionating the bottom product in a second distillation step to give an ester fraction essentially free of 1,4-cyclohexanediols and a fraction comprising at least the major part of the 1,4-cyclohexanediols, f) catalytically hydrogenating the ester fraction which is essentially free of 1,4-cyclohexanediols and g) isolating 1,6-hexanediol from the hydrogenation product in a manner known per se in a final distillation step.
Abstract:
1,6-hexanediol and .epsilon.-caprolactone are prepared from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as a by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol using oxygen or oxygen-containing gases by water extraction of the reaction mixture, by esterifying and hydrogenating a substream to give hexanediol and cyclizing 6-hydroxycaproic esters to give caprolactone.
Abstract:
N-Vinyllactams of the general formula I ##STR1## where n is from 1 to 3, are prepared by a process which comprises reaction of a lactam of the general formula II ##STR2## where n is from 1 to 3, with from 10 to 90 percent by weight of an aqueous alkali metal hydroxide solution with distillation at from 50.degree. to 250.degree. C. and from 1 to 100 mbar and with a residence time of from 0.1 to 5 hours and subsequent reaction with acetylene at from 60.degree. to 250.degree. C. and from 1 to 100 bar.
Abstract:
A process for purifying esters of tetrahydropyran-4-carboxylic acid of the formula I ##STR1## where R.sup.1 to R.sup.3 are each C.sub.1 -C.sub.4 -alkyl, and R.sup.2 and R.sup.3 are each additionally hydrogen, from mixtures produced in the reaction of butyrolactones of the formula II ##STR2## where R.sup.2 and R.sup.3 have the abovementioned meanings, and R.sup.4 is hydrogen, alkyl of 1-6 carbons or acyl of the formula --CO--R.sup.2, with alcohols of the formula R.sup.1 OH in the presence of oxide catalysts, by distillation, which entailsa) removing overhead, in a first column with 5-25 theoretical plates with a distillate pressure of 700-1100 mbar and a distillate temperature of 50.degree.-80.degree. C., an alcohol and up to 10% of the water,b) transferring the bottom product from the first column into a second column with 18-40 theoretical plates, into which a water entrainer is metered between plates 15 and 30, and is circulated, and which operates with a distillate pressure of 35-350 mbar and a distillate temperature of 18.degree.-70.degree. C., with the esters of tetrahydropyran-4-carboxylic acid being removed between plates 8 and 18 at 90.degree.-150.degree. C., and, where appropriate,c) feeding the bottom product from the second column into a third column with 5-25 theoretical plates, and returning the overhead products at a distillate pressure of 1-100 mbar and a distillate temperature of 90.degree.-140.degree. C. to the synthesis of the esters of tetrahydropyran-4-carboxylic acid.