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WO2007115897A1 - Dispositif de séparation pour la distillation de mélanges de substances - Google Patents

Dispositif de séparation pour la distillation de mélanges de substances Download PDF

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Publication number
WO2007115897A1
WO2007115897A1 PCT/EP2007/052483 EP2007052483W WO2007115897A1 WO 2007115897 A1 WO2007115897 A1 WO 2007115897A1 EP 2007052483 W EP2007052483 W EP 2007052483W WO 2007115897 A1 WO2007115897 A1 WO 2007115897A1
Authority
WO
WIPO (PCT)
Prior art keywords
distillation zone
return line
distillation
flow rate
return
Prior art date
Application number
PCT/EP2007/052483
Other languages
German (de)
English (en)
Inventor
Thomas Schwagrzinna
Bernhard Greving
Norbert Pieperbeck
Henrik Simon
Herbert Koch
Gerd KÖRSGEN
Klaus SCHÜTTER
Hubert Wolf
Original Assignee
Evonik Degussa Gmbh
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Evonik Degussa Gmbh filed Critical Evonik Degussa Gmbh
Publication of WO2007115897A1 publication Critical patent/WO2007115897A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/141—Fractional distillation or use of a fractionation or rectification column where at least one distillation column contains at least one dividing wall
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42—Regulation; Control
    • B01D3/4211—Regulation; Control of columns
    • B01D3/4216—Head stream

Definitions

  • the present invention relates to a separation device for the distillation of mixtures and a method for the distillation of mixtures using the aforementioned separation device.
  • a ternary mixture A 1 B 1 C (A: low-boiling, B: medium-boiling C; high-boiling) can be separated by separating the low-boiling product (A) at the top of the first column and the remaining higher-boiling binary mixture from the components (B) and (C) is separated in a second column.
  • distillation becomes more energetically favorable if the simplest separation is carried out first.
  • This simplest separation concerns the components with the greatest boiling distance (A) and (C).
  • this separation results in the middle boilers (B) being contained in both the distillate (A, B) and the bottom product (B, C).
  • Such distillates and bottoms must then be separated into two further columns.
  • thermodynamics circuit A more favorable from the point of view of thermodynamics circuit is a column circuit in which the distillation columns are thermally coupled together.
  • a top product is obtained in a first column, which contains the low-boiling component (A) and, for example, the medium-boiling component (B).
  • the high-boiling component (C) and medium-boiling component (B) is separated in the bottom.
  • the top product is then added to the top and / or the buoyancy part of a second column, while the bottom product of the first column is introduced into the bottom or bottom of this second column.
  • the second column then has a side draw, with which the middle boiling component (B) can be separated on.
  • the top product of the second column is the low boiling component (A).
  • the bottom product of the second column is the high boiler (C).
  • EP-A-0122367 discloses a distillation column in which two distillation zones are present. The two distillation zones are separated by a vertical partition. In this column, the substance mixture to be purified is introduced in the side stream into the first distillation zone. There, a distillation takes place and in the head of the column, the low-boiling component can be removed, while the high-boiling component can be removed from the dividing wall column in the bottom. In the second distillation zone formed by the dividing wall, the middle-boiling component is then removed.
  • a disadvantage of the aforementioned separation devices is that the control of the separation devices is very complex, since many control parameters must be coordinated.
  • One goal of such optimal control is to ensure optimum and reliable operation of the column, achieving the required product purities of the individual fractions and optimum energetic conditions.
  • the technical object of the present invention is to provide improved separators in which the product purity of the obtained products can be ensured with higher accuracy.
  • Both the first distillation zone (4) and the at least second distillation zone (5) has a head part, buoyancy part, stripping section and sump.
  • means for increasing the separation efficiency are arranged both in the first distillation zone and in the at least second distillation zone.
  • Agents may preferably be packing. However, it is also possible that
  • Distillation zone and / or at least second distillation zone are arranged.
  • the above-mentioned soils may be multi-flow due to large dimension, that is, that each floor can be equipped with two or more drainage layers, wherein the longitudinal division can be arranged arbitrarily.
  • the design of the separating device with respect to heating capacity, number of plates, arrangement of inlet and side tapping points and length of the longitudinal separation devices (subdivision) can, as known in the art, done mathematically or experimentally.
  • connection of the top part of the first distillation zone (4) with at least the second distillation zone (3) can take place through a pipeline.
  • a vertical partition (8) is arranged, the connection of the two head portions of the first and second distillation zone is effected in that the head portion of such a distillation column exclusively on the lift part (9) and / or driven part (10) of the first and at least second distillation zone (2, 3) is arranged.
  • first distillation zone (2) and the at least second distillation zone (3) are preferably separated from one another by at least one substantially vertical dividing wall (8).
  • first distillation zone (2) and the at least second distillation zone (3) are arranged in a distillation column (8).
  • the at least one partition wall (8) is arranged on the buoyancy part (9) and / or driven part (10) of the first and at least second distillation zone (2, 3). It is further preferred that the at least one partition wall (8) is arranged exclusively on the buoyancy part (9) and / or driven part (10) of the first and at least second distillation zone (2, 3).
  • a second return line (11) is preferably arranged from the top part of the at least second distillation zone (3) to the buoyancy part and / or driven part of the second distillation zone, and the second return line has at least one measuring device for determining the flow rate (13).
  • a second return line (11) from the top of the at least second distillation zone (3) to the buoyancy and / or stripping section of the second distillation zone is arranged and the second return line has at least one means for controlling the flow rate (12) and at least one measuring device Determining the flow rate (13).
  • the means for controlling the flow rate of the first Return line and the at least second return line a return divider (14), wherein the return divider at least one feed line (15) arranged at the top of the first and / or at least second distillation zone and the return divider a return line (16) arranged on the buoyancy and / or stripping section the first distillation zone and at least one further return line (17) arranged on the lift part and / or driven part of the at least second distillation zone, wherein on the return line and / or further return line, a measuring device for determining the flow rate (7,13) is arranged.
  • the device for controlling the flow rate may preferably be a valve or a slider.
  • the regulation of the flow rate may be effected by the position of a funnel in the return divider.
  • the flow through the respective return lines may be discontinuous.
  • a container can be arranged, in which the flow can be regulated in correspondingly arranged return lines via corresponding slides or valves.
  • the measuring device for determining the flow rate is a measuring system with Ultraschallmessaufêtn.
  • the reflux divider at least three hydraulically connected chambers having an inlet chamber with the inlet line and a return chamber with the return line and at least one further return chamber with the at least one other Return line is connected and the regulation of the flow through the reflux divider by a displaceable body, which is preferably a funnel.
  • a displaceable body which is preferably a funnel.
  • the material flows are adjusted by a partial body within the reflux divider by means of a magnetic coupling, whereby a pressure and vacuum-tight design is made possible.
  • the outer drive of the rotary body is effected by a rotary motor.
  • a further subject of the present invention is a process for the distillation of mixtures of substances comprising the steps: a) introduction of a substance mixture into the first distillation zone of the separation device described above and b) removal of at least one product from the buoyancy part and / or stripping part of the at least second distillation zone.
  • a second product is separated from the top of the second distillation zone.
  • a third product is withdrawn from the bottom of the second distillation zone.
  • the hydraulic load of the separating device (1) during the distillation by the material flow through the first return line (6) is set, the material flow through the first return line (6) with the measuring device for determining the flow rates is determined and the material flow is regulated by the means for regulating the flow rate.
  • hydraulic load of the separating device (1) during the distillation by the material flow through the at least second return line (11) is set, wherein the material flow through the at least second return line (11) determines with the measuring device for determining the flow rate and the material flow is regulated by means of the flow rate control device.
  • hydraulic loading is understood to be the optimal setting of the substance flows within the separating device in order to achieve an optimum separating result.
  • the means for controlling the flow rate of the first return line (6) and the at least second return line (11) is a return divider (14).
  • the reflux divider has at least one feed line (15) arranged on the top part of the first and / or at least second distillation zone.
  • a return line (6) is arranged on the buoyancy part and / or driven part of the first distillation zone and at least one further return line (11) is arranged on the buoyancy part and / or driven part of the at least second distillation zone, wherein at the return line and / or further return line a measuring device for determining the flow rate (7, 13) is arranged.
  • the separator By the method of the present invention, it is possible to operate the separator in an optimal range by a flow measurement of the return lines. In particular, it is possible to ensure a reliable operation of the column, in which the required product units of the individual fractions are achieved under optimal energetic conditions.
  • FIG. 1 shows a thermally coupled distillation column.
  • Figure 2 is a schematic representation of a separation device according to the invention, which is designed as a dividing wall column.
  • the reactant stream comprising components A, B, C (A: low-boiling components, B: medium-boiling components, C: high-boiling components) is introduced into the first column.
  • the top product of the first distillation column is transferred to the top part of the second distillation column.
  • a return line to the top of the first distillation column is arranged, which has a device for regulating the flow rate and a measuring device for determining the flow rate.
  • a feed line to the bottom of the second distillation column is arranged at the bottom of the first column, wherein here also a return line of the sump region of the second Distillation column to the bottom region of the first distillation column is arranged.
  • the low-boiling product A can be withdrawn in high purity, while the high-boiling product C can be withdrawn from the bottom region.
  • the middle-boiling product B can be withdrawn in high purity.
  • FIG. 2 shows a dividing wall column with a reflux divider.
  • the vertical partition wall mounted in the column divides the distillation column into a first distillation zone in the left-hand region of the column and a second distillation column in the right-hand region.
  • the educt stream containing A, B, C (A: low-boiling components, B: medium-boiling components, C: high-boiling components) is introduced into the first distillation zone and distilled.
  • A, B, C A: low-boiling components, B: medium-boiling components, C: high-boiling components
  • product is withdrawn and recycled via a reflux divider to the first and second distillation zones.
  • the volume flow through the two return lines is determined and controlled.
  • the high-boiling product C can be removed in high purity, while the low-boiling product A is taken from the top region of the column. From the side drive of the second distillation zone, it is possible to obtain product B as a high-purity medium-boiling component. Due to the regulation of the reflux divider and the determination of the respective reflux streams, it is possible to operate the column in an optimal energy range. In addition, it is possible to ensure a higher product purity of the separated products A, B and C by regulating the corresponding flow rate. LIST OF REFERENCE NUMBERS

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

La présente invention concerne un dispositif de séparation pour la distillation de mélanges de substances, lequel dispositif présente une première zone de distillation (2) et au moins une deuxième zone de distillation (3), le tronçon de tête de la première zone de distillation (4) étant relié au tronçon de tête de la deuxième zone de distillation (5), au moins une première conduite de retour (6) du tronçon de tête de la deuxième zone de distillation étant placée au niveau du tronçon de tête et/ou du tronçon de poussée et/ou du tronçon d'épuisement de la première zone de distillation et la première conduite de retour (6) comportant au moins un dispositif de régulation du débit (7) ainsi qu'au moins un dispositif de mesure destiné à déterminer ce débit (7). L'invention concerne également un procédé de distillation de mélanges de substances.
PCT/EP2007/052483 2006-04-10 2007-03-16 Dispositif de séparation pour la distillation de mélanges de substances WO2007115897A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006016789.9 2006-04-10
DE200610016789 DE102006016789A1 (de) 2006-04-10 2006-04-10 Trenneinrichtung zur Destillation von Stoffgemischen

Publications (1)

Publication Number Publication Date
WO2007115897A1 true WO2007115897A1 (fr) 2007-10-18

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ID=38226535

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2007/052483 WO2007115897A1 (fr) 2006-04-10 2007-03-16 Dispositif de séparation pour la distillation de mélanges de substances

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DE (1) DE102006016789A1 (fr)
WO (1) WO2007115897A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1980303B1 (fr) 2007-04-10 2018-01-24 Sulzer Chemtech AG Colonne avec tête de reflux dotée de parties de transfert de matière organisées de manière parallèle et méthode d'exploitation de la colonne
US10792583B2 (en) * 2018-03-29 2020-10-06 Uop Llc Process and apparatus for controlling the split of liquid reflux in a divided wall column

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4230533A (en) * 1978-06-19 1980-10-28 Phillips Petroleum Company Fractionation method and apparatus
EP0122367A2 (fr) * 1983-01-26 1984-10-24 BASF Aktiengesellschaft Colonne de distillation fractionnée
WO2002024300A1 (fr) * 2000-09-20 2002-03-28 Basf Aktiengesellschaft Procede et dispositif de separation par distillation de coupes c5+
EP1317947A1 (fr) * 2001-12-05 2003-06-11 Air Products And Chemicals, Inc. Procédé amelioré de distillation en discontinu
WO2004071618A1 (fr) * 2003-02-12 2004-08-26 Uop Llc Systeme de commande d'une colonne a paroi de separation

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4230533A (en) * 1978-06-19 1980-10-28 Phillips Petroleum Company Fractionation method and apparatus
EP0122367A2 (fr) * 1983-01-26 1984-10-24 BASF Aktiengesellschaft Colonne de distillation fractionnée
WO2002024300A1 (fr) * 2000-09-20 2002-03-28 Basf Aktiengesellschaft Procede et dispositif de separation par distillation de coupes c5+
EP1317947A1 (fr) * 2001-12-05 2003-06-11 Air Products And Chemicals, Inc. Procédé amelioré de distillation en discontinu
WO2004071618A1 (fr) * 2003-02-12 2004-08-26 Uop Llc Systeme de commande d'une colonne a paroi de separation

Also Published As

Publication number Publication date
DE102006016789A1 (de) 2007-10-11

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