EP1412042A2 - Verbesserter fallfilmverdampfer zur auftrennung von stoffgemischen - Google Patents
Verbesserter fallfilmverdampfer zur auftrennung von stoffgemischenInfo
- Publication number
- EP1412042A2 EP1412042A2 EP02764652A EP02764652A EP1412042A2 EP 1412042 A2 EP1412042 A2 EP 1412042A2 EP 02764652 A EP02764652 A EP 02764652A EP 02764652 A EP02764652 A EP 02764652A EP 1412042 A2 EP1412042 A2 EP 1412042A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- film evaporator
- falling film
- vapor space
- heat exchanger
- substances
- Prior art date
- Legal status (The legal status 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 status listed.)
- Withdrawn
Links
- 239000011552 falling film Substances 0.000 title claims abstract description 37
- 239000000203 mixture Substances 0.000 title claims abstract description 31
- 239000000126 substance Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 15
- 238000009833 condensation Methods 0.000 claims description 10
- 230000005494 condensation Effects 0.000 claims description 10
- 239000007792 gaseous phase Substances 0.000 claims description 5
- ZAKOWWREFLAJOT-CEFNRUSXSA-N D-alpha-tocopherylacetate Chemical compound CC(=O)OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C ZAKOWWREFLAJOT-CEFNRUSXSA-N 0.000 description 18
- ZAKOWWREFLAJOT-UHFFFAOYSA-N d-alpha-Tocopheryl acetate Natural products CC(=O)OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C ZAKOWWREFLAJOT-UHFFFAOYSA-N 0.000 description 17
- 239000000047 product Substances 0.000 description 17
- 229940042585 tocopherol acetate Drugs 0.000 description 17
- 239000000463 material Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010327 methods by industry Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000009666 routine test Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229930003427 Vitamin E Natural products 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
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
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/06—Evaporators with vertical tubes
- B01D1/065—Evaporators with vertical tubes by film evaporating
Definitions
- the present invention relates to an improved falling film evaporator for separating mixtures of substances.
- falling film evaporators have long been known in the chemical industry for the separation of mixtures of substances by distillation.
- the liquid mixture to be separated usually trickles after passing through a corresponding feed device in the form of a film on the inner walls of a heated
- Falling film evaporators are described, for example, in Billet, R.: Verdampfung 20 and their technical applications, Verlag Chemie Weinheim, 1981. Falling film evaporators are usually used to separate temperature-sensitive fluid mixtures, to concentrate solutions, etc. As a rule, falling film evaporators are used at pressures up to approx. 20 bar, in the vacuum range up to approx. 25 50 mbar. At lower pressures, the use of falling film evaporators is usually restricted, since due to the pressure loss occurring in the pipes, in the downstream vapor space and in the condenser system, the process engineering and economic outlay for the downstream vacuum system 30 increases significantly. However, these complex apparatuses are significantly more expensive in terms of investment and operation and lead to a process-technically complex process.
- a falling film evaporator for separating mixtures of substances which is characterized in that one or more heat exchangers are integrated directly into the vapor space of the falling film evaporator. Furthermore, a process for the separation of substance mixtures by feeding the substance mixture to be separated into a falling film evaporator and separating a gaseous phase from this substance mixture by a heated heat exchanger was found, which is characterized in that part of the gaseous phase is passed directly through the vapor space one or more heat exchangers condensed.
- the heat exchanger (s) arranged in the vapor space - hereinafter generally referred to as the heat exchanger system - advantageously brings about partial or complete condensation of the vapors directly in the vapor space of the falling film evaporator. This eliminates external piping to external condenser systems, which leads to significantly reduced pressure losses in the overall system consisting of falling film evaporator and condenser system.
- the substance mixture to be separated is fed via line (3) to a falling-film evaporator (1) with an internal, preferably upright, tube-bundle heat exchanger and an associated vapor space (2).
- liquid product is fed via line (4) and pump (5) into the shell-and-tube heat exchanger via a corresponding distributor device.
- the shell-and-tube heat exchanger is heated via the connections (6) and (7) with heating steam or a suitable heat transfer medium.
- the liquid phase formed collects at the lower end of the tube bundle heat exchanger and is drawn off via line (8).
- the heat exchanger system is located directly in the upper part of the vapor space. It consists of two plate capacitors (9, 11), which are separated from each other by the separating plate (10).
- the two-stage arrangement of the heat exchanger system advantageously enables partial condensation of mixtures of substances of different composition and removal of the fractions via lines (12), (13). Depending on the separation task at hand, the material flows thus obtained can be sent to the corresponding further processing.
- the residual vapor is drawn off via line (14) and vacuum system (15).
- the sump is arranged separately from the vapor space via line (8).
- This variant can prove to be particularly advantageous since it allows the concentration differences between the liquid in the vapor space and the product stream running out of the tube bundle to be exploited. Depending on the products used and selected Operating conditions with such a device may make it possible to remove almost completely the low boilers contained in the feed.
- the direct integration of the heat exchanger system into the vapor space of the falling film evaporator offers several advantages.
- the apparatus according to the invention can be used for direct condensation of the vapors formed in a process-technically simple manner.
- this design also offers the advantage of a lower pressure drop than with an arrangement of heat exchangers behind a commercially available falling film evaporator.
- the falling film evaporator according to the invention enables an economical and technically controllable use even at relatively low pressures. In general, it is suitable for pressures from about 1 mbar to 20 bar, preferably up to 1 bar. In the low-pressure range, the device can be used at pressures of up to approximately 1 mbar, preferably 3 mbar, depending on the substance system at hand, without having to operate the process-related vacuum system at great expense.
- the heat exchanger system integrated in the vapor space of the falling film evaporator has one or preferably a plurality of heat exchangers. If several heat exchangers are used, different fractions from the vapor withdrawn can be partially condensed by operating the heat exchanger appropriately.
- the condensate streams obtained in this way are preferably discharged separately and passed to corresponding further processing stages.
- Suitable heat exchangers are, for example, pipe coils or pipe bundles installed in the vapor space; plate heat exchangers are preferably used. Because of their relatively high heat transfer numbers and at the same time small pressure losses, these offer high performance and also open up the possibility of specifically adjusting the operating conditions of the individual partial condensers.
- the plate heat exchangers can be provided for condensation in cocurrent or countercurrent, depending on the process engineering task. The specific operating conditions depend on the respective material system and the separation requirements. They can be determined by the specialist through routine tests.
- the number of heat exchangers used is generally not limited, preferably two or three are used. However, more heat exchangers can also be used. As already described, it can be particularly advisable to position the sump vent separately from the vapor space.
- the concentration differences between the vapor space and the product stream running out of the tube bundle are advantageously utilized, as a result of which the separation can be made even more effective.
- a direct arrangement of the sump vent at the vapor space or in the pumping system may also be required.
- an overflow weir is installed in the vapor space, which completely or partially prevents backmixing of the liquid flowing out of the tubes of the falling film evaporator with the product stream flowing into the vapor space.
- the mixture of substances to be separated is fed to a falling film evaporator.
- a gaseous phase vapors
- a heated heat exchanger is used to expelled from the mixture of substances.
- Plate heat exchangers are preferably used in the process. These are particularly effective in the separation performance and also make it possible to achieve specific results with regard to partial condensation by means of specific operating specifications.
- the respective concrete specifications depend on the material system and the separation task and can be determined by the expert through routine tests.
- one or preferably more heat exchangers are used for the condensation. It is advisable to separate the respective condensate flows. It may be particularly advisable to design the process in such a way that the suction hood is positioned separately from the vapor space.
- the method according to the invention is particularly suitable for operations at relatively low pressures. In general, it is suitable for pressures of approximately 1 mbar to 20 bar, preferably 3 mbar to 1 bar.
- a large number of substance mixtures can be separated using the device according to the invention and the method according to the invention.
- mixtures which are sensitive to temperature and which, in addition to the product of value, contain components which, because of their concentration or the position of the phase equilibrium, boil closely to the product of value are particularly suitable. In such mixtures, partial evaporation leads to a partial transition of the product of value into the vapor stream.
- the device according to the invention can effectively minimize the losses in the valuable product.
- One example that can be mentioned here is the separation of low boilers from a material stream containing vitamin E acetate, which boil closely to the valuable product vitamin E acate.
- VEA loss 2.5% based on the incoming amount of VEA.
- the composition of the incoming product stream was 2.6% low boilers, 94.1% VEA, 1.2% high boilers and 2.1% isomers of the VEA.
- the outlet temperature of the product stream running out of the tube bundle was set to 243 ° C. at a pressure of 3 mbar.
- the outlet temperature at the first condenser was set to 180 ° C, the temperature for almost complete condensation of the remaining vapors was 150 ° C.
- the analysis of the material flow occurring at the first capacitor showed the following Composition: 13.5% low boilers, 83.9% VEA, 2.6% isomers of the VEA.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
Description
Claims
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10135716 | 2001-07-21 | ||
| DE2001135716 DE10135716A1 (de) | 2001-07-21 | 2001-07-21 | Verbesserter Fallfilmverdampfer zur Auftrennung von Stoffgemischen |
| PCT/EP2002/007609 WO2003011469A2 (de) | 2001-07-21 | 2002-07-09 | Verbesserter fallfilmverdampfer zur auftrennung von stoffgemischen |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP1412042A2 true EP1412042A2 (de) | 2004-04-28 |
Family
ID=7692726
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP02764652A Withdrawn EP1412042A2 (de) | 2001-07-21 | 2002-07-09 | Verbesserter fallfilmverdampfer zur auftrennung von stoffgemischen |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP1412042A2 (de) |
| AU (1) | AU2002328860A1 (de) |
| DE (1) | DE10135716A1 (de) |
| WO (1) | WO2003011469A2 (de) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100350209C (zh) * | 2005-11-10 | 2007-11-21 | 上海交通大学 | 降膜型滚压强化管束蒸发换热器 |
| CN102227241A (zh) * | 2008-11-27 | 2011-10-26 | 巴斯夫欧洲公司 | 蒸馏分离装置 |
| DE102010026835B4 (de) * | 2010-07-11 | 2014-07-10 | Air Liquide Global E&C Solutions Germany Gmbh | Verfahren zur Destillation von temperaturempfindlichen Flüssigkeiten |
| EP4327906A1 (de) * | 2022-08-26 | 2024-02-28 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Vorrichtung mit integriertem kondensator und abscheider |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL35201C (de) * | 1932-12-20 | |||
| EP0009251A1 (de) * | 1978-09-21 | 1980-04-02 | L. Givaudan & Cie Société Anonyme | Fraktionierverfahren und -vorrichtung |
| DE19602640A1 (de) * | 1996-01-25 | 1997-07-31 | Basf Ag | Verfahren und Verdampfer zur Verdampfung oxidationsempfindlicher Verbindungen |
| NL1013682C2 (nl) * | 1999-11-26 | 2001-05-30 | Purac Biochem Bv | Werkwijze en inrichting voor het zuiveren van een waterige oplossing van melkzuur. |
-
2001
- 2001-07-21 DE DE2001135716 patent/DE10135716A1/de not_active Withdrawn
-
2002
- 2002-07-09 WO PCT/EP2002/007609 patent/WO2003011469A2/de not_active Ceased
- 2002-07-09 EP EP02764652A patent/EP1412042A2/de not_active Withdrawn
- 2002-07-09 AU AU2002328860A patent/AU2002328860A1/en not_active Abandoned
Non-Patent Citations (1)
| Title |
|---|
| See references of WO03011469A3 * |
Also Published As
| Publication number | Publication date |
|---|---|
| DE10135716A1 (de) | 2003-02-06 |
| AU2002328860A1 (en) | 2003-02-17 |
| WO2003011469A3 (de) | 2003-04-17 |
| WO2003011469A2 (de) | 2003-02-13 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
| 17P | Request for examination filed |
Effective date: 20040223 |
|
| AK | Designated contracting states |
Kind code of ref document: A2 Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR IE IT LI LU MC NL PT SE SK TR |
|
| AX | Request for extension of the european patent |
Extension state: AL LT LV MK RO SI |
|
| RIN1 | Information on inventor provided before grant (corrected) |
Inventor name: VON ERDEN, JENS Inventor name: LAAS, HARALD Inventor name: KINNER, FRANK Inventor name: RUMPF, BERND |
|
| 17Q | First examination report despatched |
Effective date: 20040923 |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN |
|
| 18D | Application deemed to be withdrawn |
Effective date: 20050204 |