EP0379021B1 - Procédé de valorisation d'un raffinat d'une distillation extractive d'un mélange d'hydrocarbures - Google Patents

Procédé de valorisation d'un raffinat d'une distillation extractive d'un mélange d'hydrocarbures Download PDF

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Publication number
EP0379021B1
EP0379021B1 EP90100284A EP90100284A EP0379021B1 EP 0379021 B1 EP0379021 B1 EP 0379021B1 EP 90100284 A EP90100284 A EP 90100284A EP 90100284 A EP90100284 A EP 90100284A EP 0379021 B1 EP0379021 B1 EP 0379021B1
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EP
European Patent Office
Prior art keywords
raffinate
distillation column
coalescer
solvent
separation vessel
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.)
Expired - Lifetime
Application number
EP90100284A
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German (de)
English (en)
Other versions
EP0379021A1 (fr
Inventor
Gerd Emmrich
Hans-Christoph Schneider
Ulrich Rüdel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Krupp Koppers GmbH
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Krupp Koppers GmbH
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Publication of EP0379021A1 publication Critical patent/EP0379021A1/fr
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G7/00—Distillation of hydrocarbon oils
    • C10G7/08—Azeotropic or extractive distillation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S203/00—Distillation: processes, separatory
    • Y10S203/90—Particular type of heating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S210/00—Liquid purification or separation
    • Y10S210/05—Coalescer

Definitions

  • the invention relates to a process for working up the raffinate of an extractive distillation of hydrocarbon mixtures, in which N-substituted morpholines, the substituents of which have no more than seven carbon atoms, are used as the selective solvent, the lower-boiling constituents of the hydrocarbon mixture serving as the feed product being used as raffinate withdrawn overhead from the extractive distillation column and the raffinate then distilled to recover the solvent residues contained therein and the resulting bottom product with a certain solvent content is withdrawn from the raffinate distillation column and separated into a light and a heavy phase in a separating container, whereupon the heavy phase is reintroduced into the extractive distillation column and the light phase into the raffinate distillation column.
  • the extractive distillation process described above has been known for a number of years and can be used for the separation of hydrocarbon mixtures of different compositions, for example for the separation of aromatics and non-aromatics or for the separation of olefins or diolefins and paraffins.
  • the process has become particularly useful using N-formylmorpholine as a selective solvent for obtaining highly pure aromatics proven.
  • the bottom product withdrawn from the extractive distillation column is normally passed into a downstream stripping column in which the hydrocarbons contained in it as extract are separated from the solvent by distillation.
  • the solvent is then withdrawn from the bottom of the stripping column and returned to the extractive distillation column for reuse.
  • the solvent is usually introduced or reintroduced at the top of the extractive distillation column.
  • the invention is therefore based on the object of eliminating this disadvantage.
  • coalescer In the coalescer, the very fine droplets of the heavy phase can unite to form large drops, which can then sink down without difficulty as a result of their higher sinking speed in the separating container.
  • a coalescer which is particularly suitable for carrying out the method according to the invention and its mode of action will be discussed below in connection with FIGS. 2 and 3.
  • the bottom product with a solvent content of 20 to 75% by weight is drawn off from the raffinate distillation column and cooled to a temperature of 20 to 70 ° C. before entering the coalescer.
  • the solvent content of the bottom product of the raffinate distillation can in this case be controlled via the bottom temperature or the temperature of the column heating at the bottom of the raffinate distillation column, since there is a clear relationship between the solvent content and the bottom temperature such that the bottom temperature rises with increasing solvent content, the bottom temperature setting is of course dependent on the boiling point of the solvent used and the composition of the hydrocarbon mixture to be worked up in the raffinate distillation column.
  • benzene is obtained from a crude benzene fraction obtained from pyrolysis gasoline by extractive distillation with N-formylmorpholine and a solvent content in the bottom product of the raffinate distillation column of 50% by weight
  • a bottom temperature is established.
  • the content of the same solvent in the bottom product is 75% by weight, the bottom temperature is approximately 125 ° C.
  • the flow diagram shown in FIG. 1 contains only the parts of the system that are absolutely necessary for the process explanation, while auxiliary devices such as pumps, circulation cookers, heat exchangers etc. are not shown.
  • the hydrocarbon mixture serving as the feed product which may already have been subjected to pre-distillation, is introduced through line 1 into the central part of the bottomed extractive distillation column 2.
  • the feed product is usually heated to just below the boiling point so that it evaporates immediately when it enters the extractive distillation column.
  • the selective solvent used is introduced at the top into the extractive distillation column 2 and flows down over the trays of this column, taking up the vaporous hydrocarbons of the extract.
  • the lower-boiling hydrocarbons which form the raffinate phase escape through line 4 at the top of the column and pass through this line into the middle part of the raffinate distillation column 19 provided with packing or trays.
  • the liquid bottom product of the extractive distillation column 2 consists of the solvent and the hydrocarbons of the extract dissolved therein and is withdrawn through line 5 from the extractive distillation column 2 and reaches the stripping column 6, in which these hydrocarbons are separated from the selective solvent by distillation.
  • the solvent is removed from the bottom of the column through line 7 and flows back through line 3 into the extractive distillation column 2 while the hydrocarbons to be extracted escape overhead from the stripping column 6 and pass through line 8 into column 9, in which their further Separation takes place.
  • the higher-boiling components can be drawn off through line 10 and the lower-boiling components can be drawn off through line 11.
  • the branch line 12 is provided in the area of the line 7, through which a partial amount of the solvent can reach the regeneration device 14 when the valve 13 is in the appropriate position.
  • the regenerated solvent is through line 15 again returned to the circuit (line 7), while the separated impurities are removed from the regeneration device through line 16.
  • the line 17 is finally used to supply fresh solvent.
  • the bottom product obtained in the raffinate distillation column 19 is drawn off via line 21 with a solvent content of 20 to 75% by weight, while hydrocarbons of the raffinate with a solvent content of less than 10 ppm are removed via line 2o from the raffinate distillation column 19 .
  • the withdrawn sump product passes via line 21 into the cooler 22, in which it undergoes the necessary cooling.
  • it is introduced via line 29 into the coalescer 3o, which is combined with the separating container 23 to form a structural unit.
  • the bottom product from the coalescer 3o therefore enters directly into the upper part of the separating tank 23, in which the interface controller 24 is installed in the central region.
  • the cooler 22 Since the amount of sump product flowing off via the line 21 is relatively small, the cooler 22 will not always be necessary for the cooling thereof required. If necessary, it is rather also possible to dispense with this cooler and to cool the bottom product in line 21 and in the separating container 23 in that the latter are not insulated or are equipped with a cooling jacket. Excessive cooling of the bottom product to a temperature below 20 ° C. is not appropriate, because it causes the heating energy requirement in the raffinate distillation column 19 and the extractive distillation column 2 would be increased unnecessarily. At a temperature between 2o and 7o ° C, the desired separation of the introduced bottom product into an upper and a lower phase takes place in the separating tank. The different composition of these two phases has already been mentioned above.
  • the withdrawal of the heavy phase (lower phase) from the separating tank 23 is controlled by the interface controller 24. This is done in such a way that the position of the interface between the heavy and the light phase influences the position of the interface controller 24, which is attached to a joint in a freely movable manner. As soon as the heavy phase has accumulated in the lower part of the separating tank 23 to such an extent that the interface between the heavy and light phases is at the same level as the interface controller 24, it assumes the horizontal position shown in the figure and actuates it when this position is reached Via the pulse line 27, the actuator 28 of the valve 26 in such a way that it is opened.
  • the valve 26 Since the valve 26 is installed in the line 25, the heavy phase is drawn off from the separating container 23 and can be combined with the solvent flowing in the line 3 via this line. If, on the other hand, the separating layer between the heavy and light phases in the separating container continues to decrease, the position of the separating layer regulator 24 changes accordingly downward and the valve 26 is closed or throttled in the manner described. The light phase (upper phase) is meanwhile removed from the separating tank 23 via the line 18 and returns to the bottom of the raffinate distillation column 19. It deviates from the circuit shown in the flow diagram of course, it is also possible not to combine the heavy phase drawn off through line 25 with the solvent in line 3, but rather to introduce it separately into the upper part of the extractive distillation column 2.
  • coalescer 3o which is connected to the associated separating container 23 to form a structural unit. It can be seen that the coalescer 3o is flanged onto the upper part of the separating container 23 so that the bottom product in the coalescing 3o can flow out of the raffinate distillation column 19 directly into the upper part of the separating container 23.
  • the reference symbols 18, 25 and 29 mark the connections for the corresponding lines and the reference symbol 24 the connection for the interface controller.
  • Fig. 3 finally shows a section through the coalescer 3o in the plane AB of Fig. 2. It can be seen in the figure that the interior of the coalescer 3o in this case is completely filled with corrugated metal plates 31 arranged one above the other. These corrugated iron plates 31 are arranged in the coalescer 3o in such a way that their grooves 32 run parallel to the longitudinal direction of the coalescer 3o. In addition, the corrugated metal plates 31 have a gradient of approximately 1% in the direction of the inlet opening to the separating container 23, so that the bottom product located in the coalescer 30 can easily flow into the separating container 23.
  • the corrugated metal plates 31 should preferably consist of pickled carbon steel because this material guarantees good wettability.
  • the channel 32 of a corrugated iron plate 31 is shown in FIG. 3 as a detailed illustration. The depth a of the grooves 32 should preferably be 20 mm.
  • coalescer 30 and the separating container 23 are combined to form one structural unit, which is undoubtedly the preferred embodiment. If special operational circumstances require it, it is also possible to arrange the coalescer 30 and the separating container 23 separately from one another.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Claims (2)

  1. Procédé d'affinage du produit de raffinage d'une distillation extractive de mélanges d'hydrocarbures dans laquelle on utilise comme solvant sélectif des N-morpholines substituées dont les substituants ne présentent pas plus de sept atomes de C, étant entendu que les fractions constitutives du mélange d'hydrocarbures servant de produit de mise en oeuvre dont le point d'ébullition est relativement bas, sont soutirées au sommet de la colonne de distillation extractive sous la forme d'un produit de raffinage, et qu'ensuite le produit de raffinage est distillé afin de récupérer les restes de solvant qu'il contient, et que le produit recueilli à la base de la colonne de distillation de raffinage en est soutiré dans ces conditions avec une certaine teneur en solvant et séparé dans un récipient séparateur en une phase légère et une phase plus lourde, à la suite de quoi la phase plus lourde est réintroduite dans la colonne de distillation extractive et la plus légère dans la colonne de distillation de raffinage,
    caractérisé par le fait que l'on fait circuler le produit recueilli à la base de la colonne de distillation du produit de raffinage, avant son introduction dans le récipient séparateur (23), par un dispositif (30) de coalescence dont le volume intérieur est complètement comblé par des plaques (31) en tôle ondulée placées l'une par dessus l'autre, composées d'acier au carbone décapé, tandis que les plaques (31) en tôle ondulée sont disposées de manière telle que leurs rainures (32) s'étendent parallèlement au sens de la longueur du dispositif (30) de coalescence et accusent au surplus une légère pente en direction de l'orifice de sortie.
  2. Dispositif de coalescence avec des infrastructures placées l'une par dessus l'autre en vue de la mise en oeuvre du procédé suivant la revendication 1,
    caractérisé par le fait que ledit dispositif est regroupé en une unité cohérente de construction avec le récipient séparateur (23), tandis que le dispositif (30) de coalescence est monté par bride sur la partie supérieure du récipient séparateur (23) et que les plaques (31) en tôle ondulée, dont les rainures (32) qui s'étendent parallèlement au sens de la longueur du dispositif (30) de coalescence ont une profondeur de 20 mm, accusent une pente de 1 % en direction de l'orifice d'entrée du récipient (23) de décantation.
EP90100284A 1989-01-20 1990-01-08 Procédé de valorisation d'un raffinat d'une distillation extractive d'un mélange d'hydrocarbures Expired - Lifetime EP0379021B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3901587A DE3901587A1 (de) 1989-01-20 1989-01-20 Verfahren zur aufarbeitung des raffinates einer extraktivdestillation von kohlenwasserstoffgemischen
DE3901587 1989-01-20

Publications (2)

Publication Number Publication Date
EP0379021A1 EP0379021A1 (fr) 1990-07-25
EP0379021B1 true EP0379021B1 (fr) 1993-09-15

Family

ID=6372451

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Application Number Title Priority Date Filing Date
EP90100284A Expired - Lifetime EP0379021B1 (fr) 1989-01-20 1990-01-08 Procédé de valorisation d'un raffinat d'une distillation extractive d'un mélange d'hydrocarbures

Country Status (7)

Country Link
US (1) US5031754A (fr)
EP (1) EP0379021B1 (fr)
JP (1) JP2768528B2 (fr)
KR (1) KR0141364B1 (fr)
CA (1) CA2008029C (fr)
DE (2) DE3901587A1 (fr)
ES (1) ES2047158T3 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4101848A1 (de) * 1991-01-23 1992-07-30 Krupp Koppers Gmbh Verfahren zur abtrennung von aromaten aus kohlenwasserstoffgemischen beliebigen aromatengehaltes
DE4109632A1 (de) * 1991-03-23 1992-09-24 Krupp Koppers Gmbh Verfahren zur abtrennung von aromaten durch extraktivdestillation
EP0666767B1 (fr) * 1992-10-28 2000-03-08 Chevron Chemical Company LLC Production de benzene tres pur par distillation extractive
US9005405B2 (en) 2012-03-01 2015-04-14 Cpc Corporation, Taiwan Extractive distillation process for benzene recovery
US9221729B1 (en) * 2015-02-23 2015-12-29 Allnew Chemical Technology Company Extractive distillation for aromatics recovery
CN116574531B (zh) * 2023-07-13 2023-10-27 大庆亿鑫化工股份有限公司 一种生产石油醚的炉式装置和生产工艺

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA512198A (fr) * 1955-04-26 H. Engel Karl Distillation azeotropique d'huiles d'hydrocarbures
US2376870A (en) * 1941-03-28 1945-05-29 Allied Chem & Dye Corp Azeotropic distillation of hydro-carbon oils
US4081355A (en) * 1970-08-12 1978-03-28 Krupp-Koppers Gmbh Process for recovering highly pure aromatics from a mixture of aromatics and non-aromatics
US3844902A (en) * 1973-04-02 1974-10-29 A Vickers Combination of extractive distillation and liquid extraction process for separation of a hydrocarbon feed mixture
US4191615A (en) * 1974-12-17 1980-03-04 Krupp-Koppers Gmbh Process for operating extraction or extractive distillation _apparatus
US4056371A (en) * 1976-02-23 1977-11-01 Diemer Jr R Bertrum Method for separating immiscible fluids of different density
US4032332A (en) * 1976-09-03 1977-06-28 Kennecott Copper Corporation Process for increasing the rate of copper metal production in a quinolic extraction system
DE2931012A1 (de) * 1979-07-31 1981-02-26 Metallgesellschaft Ag Verfahren zur gewinnung von reinbenzol
US4498980A (en) * 1983-02-14 1985-02-12 Union Carbide Corporation Separation of aromatic and nonaromatic components in mixed hydrocarbon feeds
DE3409030A1 (de) * 1984-03-13 1985-09-19 Krupp Koppers GmbH, 4300 Essen Verfahren zur abtrennung von aromaten aus kohlenwasserstoffgemischen beliebigen aromatengehaltes
US4781820A (en) * 1985-07-05 1988-11-01 Union Carbide Corporation Aromatic extraction process using mixed polyalkylene glycols/glycol ether solvents
US4664754A (en) * 1985-07-18 1987-05-12 General Electric Company Spent liquid organic solvent recovery system
US4897206A (en) * 1988-11-30 1990-01-30 Facet Quantek, Inc. Bidirectionally corrugated plate separator for fluid mixtures
US4877594A (en) * 1988-12-13 1989-10-31 J. R. Simplot Co. Purification of phosphoric acid

Also Published As

Publication number Publication date
ES2047158T3 (es) 1994-02-16
US5031754A (en) 1991-07-16
JP2768528B2 (ja) 1998-06-25
CA2008029C (fr) 1996-11-19
EP0379021A1 (fr) 1990-07-25
KR900011881A (ko) 1990-08-02
CA2008029A1 (fr) 1990-07-20
DE59002673D1 (de) 1993-10-21
DE3901587A1 (de) 1990-07-26
KR0141364B1 (ko) 1998-06-15
JPH02232295A (ja) 1990-09-14

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