Abstract:
A process for the production of higher (meth)acrylic esters, comprises an esterification step of esterifying (meth)acrylic acid with an alcohol to obtain a crude (meth)acrylic ester, the (meth)acrylic acid containing trace amounts of acetic acid; and purification steps of purifying the crude (meth)acrylic ester. The purification steps comprise introducing crude (meth)acrylic ester into the side of a low boiler column with a rectifying section disposed above the feed point of the crude (meth)acrylic ester and a stripping section disposed below the feed point; withdrawing purified (meth)acrylic ester from the low boiler column; withdrawing a low boiler fraction from the top of the low boiler column, the low boiler fraction comprising alcohol and acetic ester and less than 10 wt.-% of (meth)acrylic ester; directing the low boiler fraction to an acetate column, the acetate column being operated at a pressure at least 50 mbar higher than the low boiler column pressure, and separating the low boiler fraction into an alcohol fraction withdrawn at the top of the acetate column and an acetic ester fraction withdrawn at the bottom of the acetate column; and recycling the alcohol fraction at least partially to the esterification step; the process comprising no recycle from the acetate column to the low boiler column. The process provides an effective and economically viable process for preparing higher (meth)acrylic esters with a low acetate content.
Abstract:
A process for continuously preparing the tert-butyl ester of an ethylenically unsaturated carboxylic acid, by a) reacting an ethylenically unsaturated carboxylic acid with isobutene in the presence of an acidic catalyst to give an esterification mixture; b) removing the acidic catalyst; c) removing low-boiling components; and d) supplying a tert-butyl ester-comprising liquid to a distillation apparatus and subjecting it to purifying distillation in the distillation apparatus, where d1) in the distillation apparatus the tert-butyl ester-comprising liquid is separated into a tert-butyl ester-comprising gaseous top product and a carboxylic acid-comprising liquid bottom product; d2) the tert-butyl ester-comprising gaseous top product is at least partly condensed and the condensate is recycled partly as reflux to the distillation apparatus; d3) the carboxylic acid-comprising liquid bottom product is recycled at least partly to step a); d4) carboxylic acid-comprising liquid bottom product is drawn off and passed to a heater; a superheated, liquid recycle stream is taken from the heater; and the superheated recycle stream is let down into the distillatiuon apparatus; and d5) at least in the top region of the distillation apparatus, the distillation apparatus walls in contact with the vapor, at least in sub-regions, are heated and/or thermally insulated. In the course of the process, the separation of the tert-butyl ester from unreacted carboxylic acid is carried on with a particularly low level of accompanying polymerization both of the tert-butyl ester and of the carboxylic acid.
Abstract:
Process for isolating pure 2-ethylhexyl acrylate or pure 2-propylheptyl acrylate from the corresponding crude alkyl acrylate by distillation, wherein the process is carried out in a dividing wall column (1) which has separation-active internals and vaporizer (7) and in which a dividing wall (8) is arranged in the longitudinal direction of the column to form an upper joint column region (9), a lower joint column region (14), an inflow section (10, 12) having a side feed point (2) and an offtake section (11, 13) having a side offtake point (3), the column has a number of theoretical plates in the range from 10 to 60, where the number of theoretical plates of the dividing wall column (1) relates to the sum of the theoretical plates in the joint upper column region (9), the joint lower column region (14) and the inflow section (10, 12), the side feed point (2) for the corresponding crude alkyl acrylate is arranged at a theoretical plate in the region commencing at least two theoretical plates above the bottommost theoretical plate and ending at least two theoretical plates below the uppermost theoretical plate, the side offtake point (3) for the pure 2-ethylhexyl acrylate or pure 2-propylheptyl acrylate is arranged at a theoretical plate in the region commencing at least two theoretical plates above the bottommost theoretical plate and ending at least two theoretical plates below the uppermost theoretical plate and the dividing wall (8) is arranged in the column in the region commencing at least one theoretical plate above the bottommost theoretical plate and ending at least one theoretical plate below the uppermost theoretical plate, where the ratio of amount of liquid at the upper end of the dividing wall (8) going to the enrichment section (10) and the stripping section (11) of the column is set in the range from 1:0.2 to 1:5.
Abstract:
A process for continuously preparing a butyl acrylate H2C═CH—C(═O)OR, with R=n-butyl or isobutyl, wherein aqueous 3-hydroxypropionic acid is converted under dehydrating and esterifying conditions in the presence of the corresponding butanol R—OH in a reactor with a rectification column and butyl acrylate formed, unconverted butanol and water used and formed are distilled off overhead as a ternary azeotrope, after separation into a liquid aqueous phase and liquid organic phase each of the aqueous and organic phases is at least partly discharged, and the organic phase comprising the butyl acrylate and the butanol is subjected to distillative separation.
Abstract:
A process for isolating pure butyl acrylate from crude butyl acrylate, which is carried out in a dividing wall column having separation-active internals and a vaporizer, and in which: a dividing wall is arranged in a longitudinal direction of the column to form an upper joint column region, a lower joint column region, an inflow section having a side feed point and an offtake section having a side offtake point; a ratio of an amount of liquid at an upper end of the dividing wall going to an enrichment section and a stripping section of the column is set in the range from 1:0.2 to 1:5; and a ratio of an amount of vapor streams at a lower end of the dividing wall going to the stripping section and the enrichment section of the column is set in a range from 1:0.5 to 1:2.0.
Abstract:
A continuous process for preparing (meth)acrylates of C10-alcohol mixtures by reaction of glacial (meth)acrylic acid with an isomer mixture of C10-alcohols composed of 2-propylheptanol as the main isomer and at least one of the C10-alcohols 2-propyl-4-methylhexanol, 2-propyl-5-methylhexanol, 2-isopropylheptanol, 2-isopropyl-4-methylhexanol, 2-isopropyl-5-methylhexanol and/or 2-propyl-4,4-dimethylpentanol, and the use of a diester of dicarboxylic acids which have been esterified with N-oxyl-containing compounds as polymerization inhibitors in such a process.
Abstract:
The invention relates to a centrifugal droplet separator for separating liquid droplets out of a gas stream, comprising a shell (1) having a circular cross section and a vertical longitudinal axis (11), an upper hood (2) that bounds the shell (1) at the top and has a gas exit port (7) for the gas stream cleaned in the centrifugal droplet separator, a drip plate (8) disposed beneath the gas exit port (7), a lower hood (10) that bounds the shell (1) at the bottom and has a liquid exit port (4) for removal of the deposited liquid droplets, and an inlet (3) that opens tangentially into the shell (1) for supply of the gas stream,
wherein there are at least two nozzles (9) for feeding a stabilizer liquid into the interior of the centrifugal droplet separator, the respective nozzle outlet (15) of which is disposed between the tangential inlet (3) and the drip plate (8) in vertical direction, where the main spraying direction (12) of the nozzles (9) is directed upward at an internal angle of 0 to 60° relative to the vertical longitudinal axis (11).
The invention additionally also relates to a method of separating liquid droplets out of a gas stream in such a centrifugal droplet separator.
Abstract:
The present invention relates to a continuous process for obtaining 2-ethylhexyl acrylate (2-EHA) from a mixture (1) that is liquid under an absolute pressure in the range from 0.5 to 100 bar and has a temperature in the range from 0 to 300° C., comprising 2-EHA, at least one high boiler, at least one homogeneous catalyst, and at least one low boiler, wherein the mixture (1) is depressurized by a pressure-maintenance device (3) to an absolute pressure level in the range from 0.1 to 10 bar, wherein the resulting two-phase gas/liquid mixture (16) is continuously supplied to a helical-tube evaporator (4) in which, at a temperature in the range from 50 to 300° C., the 2-EHA content of the liquid phase of the two-phase gas/liquid mixture is reduced by partial evaporation, this being accompanied by a parallel increase in the 2-EHA content of the gas phase of the two-phase gas/liquid mixture, and the two phases are discharged in the form of a resulting two-phase gas/liquid output stream (17).
Abstract:
The invention relates to an apparatus for carrying out mass transfer processes, comprising a column having at least two inlet pipes for introducing a gaseous phase, where separation-active internals are accommodated in the column and a column section extends from the at least two inlet pipes to the separation-active internals, in which section a coverage of a cross-sectional area of the column is less than 25%, based on the total cross-sectional area, and where the at least two inlet pipes have a height offset which corresponds to not more than three times an inlet pipe diameter and the at least two inlet pipes are at an angle (α) of from 60° to 150° to one another and have asymmetry with respect to one another. The invention further relates to a use of the apparatus and also a method for designing the apparatus.
Abstract:
Process for isolating pure tert-butyl (meth)acrylate from crude tert-butyl (meth)acrylate by distillation, wherein the process is carried out in a dividing wall column (1) which has separation-active internals and vaporizer (7) and in which a dividing wall (8) is arranged in the longitudinal direction of the column to form an upper joint column region (9), a lower joint column region (14), an inflow section (10, 12) having a side feed point (2) and an offtake section (11, 13) having a side offtake point (3), the column has a number of theoretical plates in the range from 20 to 80, where the number of theoretical plates of the dividing wall column (1) relates to the sum of the theoretical plates in the joint upper column region (9), the joint lower column region (14) and the inflow section (10, 12), the side feed point (2) for the crude tert-butyl (meth)acrylate is arranged at a theoretical plate in the region commencing at least two theoretical plates above the bottommost theoretical plate and ending at least two theoretical plates below the uppermost theoretical plate, the side offtake point (3) for the pure tert-butyl (meth)acrylate is arranged at a theoretical plate in the region commencing at least two theoretical plates above the bottommost theoretical plate and ending at least two theoretical plates below the uppermost theoretical plate and the dividing wall (8) is arranged in the column in the region commencing at least one theoretical plate above the bottommost theoretical plate and ending at least one theoretical plate below the uppermost theoretical plate, where the ratio of amount of liquid at the upper end of the dividing wall (8) going to the enrichment section (10) and the stripping section (11) of the column is set in the range from 1:0.2 to 1:5.