EP0418622B1 - Procédé pour la séparation de composés aromatiques - Google Patents

Procédé pour la séparation de composés aromatiques Download PDF

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Publication number
EP0418622B1
EP0418622B1 EP90116818A EP90116818A EP0418622B1 EP 0418622 B1 EP0418622 B1 EP 0418622B1 EP 90116818 A EP90116818 A EP 90116818A EP 90116818 A EP90116818 A EP 90116818A EP 0418622 B1 EP0418622 B1 EP 0418622B1
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Prior art keywords
solvent
benzene
temperature
process according
separation
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EP90116818A
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German (de)
English (en)
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EP0418622A3 (en
EP0418622A2 (fr
Inventor
Manfred Jeschke
Hans-Joachim Dr. Krämer
Jörg-Uwe Michel
Hermann Vechtel
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Erdoelchemie GmbH
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Erdoelchemie GmbH
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    • 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

Definitions

  • the invention relates to a process for the separation and simultaneous purification of aromatics from aromatic hydrocarbons.
  • Starting materials are mixtures of aromatic and non-aromatic hydrocarbons, from which the pure aromatics cannot be separated or can only be separated with unreasonably high effort because of the boiling point and because of the formation of azeotropic mixtures by simple thermal distillation.
  • aromatics to be removed include benzene, toluene and the xylene isomers, both together and individually. Mixtures of this type to be separated are obtained, for example, in refineries and petrochemical plants.
  • N-substituted morpholines such as N-formyl morpholine (NFM); N-substituted Pyrrolidones such as N-methyl-pyrrolidone (NMP); Tetrahydrothiophene dioxide (sulfolane); Dimethylformamide (DMF).
  • NFM N-formyl morpholine
  • NMP N-substituted Pyrrolidones
  • NMP N-methyl-pyrrolidone
  • Tetrahydrothiophene dioxide sulfolane
  • DMF Dimethylformamide
  • the non-extracted non-aromatics are drawn off in gaseous form at the top of the extractive distillation column, while a mixture of the selective solvent and the aromatics is taken off as the bottom product.
  • This bottom product is fed to a downstream column (stripper), where the pure aromatic product is removed as the top product and the regenerated selective solvent as the bottom product by distillation.
  • FIG. 1 shows the following apparatus: An extractive distillation column (I), a raffinate column (II), a stripper (III), two condensers (IV) and (V), a cooler (VI), two bottom circulation heaters (VII) and (VIII) and three heat exchangers (IX), (X) and (XI).
  • the figure shows the following material flows: The mixture of aromatics and non-aromatics (1) to be used, the (regenerated) selective solvent (2) to be used, the gaseous raffinate (3), the liquid raffinate reflux (4), the raffinate removal (5), the selective solvent (6) loaded with the extracted aromatic (s), the gaseous aromatic (7), the reflux of the aromatic (s) (8), the aromatic removal (9).
  • the method is briefly described using the figure as follows:
  • the feed mixture (1) is fed in at a temperature just below its boiling point under the operating conditions of (I) in (I).
  • the selective solvent (2) is fed in at the top of (I). It flows down over the internals of (I), taking up the aromatics.
  • the non-aromatic hydrocarbons pass in gaseous form, for example through a chimney floor according to (II), where the raffinate to be taken off as the top product is freed of any entrained solvent vapors.
  • (II) can be directly connected to (I) via the chimney tray shown in Figure 1 or can be integrated into the process as a completely separate column.
  • the regenerated selective solvent is taken from (III) at the bottom, partly pumped through the bottom circulation heater (VIII) and partly as (2) via the heat exchangers (IX), (X) and optionally (XI) and a cooler ( VI) fed again (I).
  • the heating energy introduced into the process via (VIII) is used to cover the energy requirement of (I) via (IX) and the energy requirement of (II) via (X).
  • sensible heat can still be given to an external consumer via (XI).
  • the temperature of (2) required for feeding into (I) is set in (VI).
  • the aromatics content in the raffinate is influenced by the temperature and the amount of the solvent used in the extractive distillation column.
  • a feed temperature for the selective solvent which is above the working temperature of the extractive column at the feed point, has proven useful. If the temperature of the selective solvent is reduced further, the aromatic content in the raffinate decreases, but at the same time a higher raffinate content dissolves in the solvent, which can only be compensated for by a higher evaporation rate in the bottom circulation of the extractive distillation column. Similar effects are brought about by increasing the amount of solvent.
  • a process for the separation of aromatics from aromatics-containing hydrocarbons by extractive distillation using a selective solvent is characterized in that the selective solvent is fed into the extractive distillation column at a temperature which is equal to that at the feed point up to 40 ° C. is below the temperature at the feed point in the column, and at the same time the amount of solvent is reduced by 10 to 50% of the standard amount of solvent, the decrease in solvent temperature and the decrease in amount of solvent being directly correlated.
  • the temperature at the feed point in the column is generally the condensation temperature of the raffinate.
  • the reduction in the solvent temperature is preferably 5 to 40 ° C. and the reduction in the amount of solvent is 15 to 45% of the standard amount mentioned, the two values correlating directly with one another.
  • the standard amount of solvent to which the reduction applies depends on the selectivity of these solvents. These relationships are known to the person skilled in the art. For example, 5.5 to 7.5 t / t of benzene, often 5.7 to 6.5 t of NMP / t of benzene, can be used to separate benzene.
  • the maximum lowering of the solvent temperature can be less than at normal pressure.
  • N-substituted morpholines N-substituted pyrrolidones, tetrahydrothiophene dioxide, DMF or a mixture of several of them are preferably used, particularly preferably N-formyl-morpholine or N-methyl-pyrrolidone (NMP). .
  • the process according to the invention is applied in a special way to the joint production of benzene, toluene and the xylene isomer (BTX aromatics), to the joint production of benzene and toluene and to the production of benzene from corresponding distillation cuts; in a particularly preferred manner, the method according to the invention is applied to the extraction of benzene from a so-called benzene cut.
  • NMP in the production of benzene is particularly important.
  • the extractive distillation and regeneration of the solvent in the stripper can generally be carried out under normal pressure. However, they are preferably carried out independently of one another under reduced pressure. When removing benzene, operating data in the range from 150-400 mbar and 35-65 ° C. top temperature are advantageously selected for the extractive distillation column.
  • the lowering of the temperature of the selective solvent to be fed in, starting from a conventional procedure is reduced in small steps in order to maintain the stable mode of operation of the column.
  • the amount of solvent is reduced to the same extent.

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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)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Claims (8)

  1. Procédé de séparation de carbures aromatiques d'hydrocarbures contenant des carbures aromatiques par distillation extractive et utilisation d'un solvant sélectif, caractérisé en ce que le solvant sélectif est introduit dans la colonne de distillation extractive à une température égale à inférieure jusqu'à 40°C à la température régnant dans la colonne à l'endroit d'alimentation, et en ce que simultanément la quantité du solvant est diminuée de 10 à 50 % par rapport à la quantité standard de solvant, l'abaissement de la température du solvant et la diminution de la quantité de solvant étant en corrélation directe.
  2. Procédé selon la revendication 1, caractérisé en ce que l'abaissement de la température du solvant est compris entre 5 et 40°C et la diminution de la quantité de solvant entre 15 et 45 % et les deux valeurs sont directement corrélées.
  3. Procédé selon la revendication 1, caractérisé en ce qu'on utilise, comme solvant sélectif, des morpholines N-substituées, des pyrrolidones N-substituées, du dioxyde de tétrahydrothiophène, du diméthylformamide ou un mélange de plusieurs d'entre eux.
  4. Procédé selon la revendication 1, caractérisé en ce qu'on procède à la séparation commune de benzène, de toluène et des isomères de xylène (carbures aromatiques BTX), à la séparation commune de benzène et de toluène ou à la séparation de benzène à partir de coupes de distillation appropriées en tant que séparation de carbures aromatiques.
  5. Procédé selon la revendication 4, caractérisé en ce qu'on procède à l'extraction de benzène à partir d'une coupe de distillation de benzène en tant que séparation de carbures aromatiques.
  6. Procédé selon la revendication 5, caractérisé en ce que lors de la séparation de benzène on utilise de la N-méthylpyrrolidone comme solvant sélectif.
  7. Procédé selon la revendication 6, caractérisé en ce que la quantité de solvant L en t/h, la température du solvant T à l'entrée de la colonne de distillation extractive en °C et la production de benzène E en t/h pour une production de benzène comprise entre 5 et 50 t/h, de préférence entre 10 et 30 t/h, sont liées de la façon suivante :

    L = a · T + b · E - c,
    Figure imgb0006

    où les facteurs a, b, c prennent les valeurs
       a = 1,1-1,2,
       b = 3,5-4,5 et
       c = 20-40.
  8. Procédé selon la revendication 5, caractérisé en ce que la colonne de distillation extractive fonctionne pour une pression en tête comprise entre 150 et 400 mbar et une température en tête comprise entre 35 et 65°C.
EP90116818A 1989-09-16 1990-09-01 Procédé pour la séparation de composés aromatiques Expired - Lifetime EP0418622B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3930992A DE3930992A1 (de) 1989-09-16 1989-09-16 Verfahren zur abtrennung von aromaten
DE3930992 1989-09-16

Publications (3)

Publication Number Publication Date
EP0418622A2 EP0418622A2 (fr) 1991-03-27
EP0418622A3 EP0418622A3 (en) 1992-11-04
EP0418622B1 true EP0418622B1 (fr) 1994-11-30

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Family Applications (1)

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EP90116818A Expired - Lifetime EP0418622B1 (fr) 1989-09-16 1990-09-01 Procédé pour la séparation de composés aromatiques

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EP (1) EP0418622B1 (fr)
DE (2) DE3930992A1 (fr)
ES (1) ES2064569T3 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1172886C (zh) 2001-06-29 2004-10-27 中国石油化工股份有限公司 一种抽提蒸馏分离芳烃的方法及使用的复合溶剂
FR2843403B1 (fr) * 2002-08-08 2007-08-24 Totalfinaelf France Procede et dispositif de purification d'une coupe petroliere
CA2953398C (fr) * 2014-07-01 2023-06-13 Anellotech, Inc. Procedes pour la conversion de biomasse en btx a faible teneur en soufre, en azote et en olefines par l'intermediaire d'un procede de pyrolyse catalytique rapide

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1568940C3 (de) * 1966-12-19 1978-12-07 Krupp-Koppers Gmbh, 4300 Essen Verfahren zur Abtrennung von Aromaten aus Kohlenwasserstoffgemischen beliebigen Aromatengehaltes
DE2026693C3 (de) * 1970-06-01 1973-11-29 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zur Gewinnung von Rein benzol durch Extraktivdestillation
DE3032780A1 (de) * 1980-08-30 1982-04-15 Krupp-Koppers Gmbh, 4300 Essen Verfahren zur aufarbeitung des sumpfproduktes von extraktivdestillationsprozessen zur gewinnung reiner kohlenwasserstoffe
DE3409307A1 (de) * 1984-03-14 1985-09-19 Krupp Koppers GmbH, 4300 Essen Verfahren zur abtrennung von aromaten aus kohlenwasserstoffgemischen beliebigen aromatengehaltes
US4556404A (en) * 1984-09-19 1985-12-03 Air Products And Chemicals, Inc. Split-column extractive distillation
DE3602240A1 (de) * 1986-01-25 1987-07-30 Krupp Koppers Gmbh Verfahren zur abtrennung von aromaten aus kohlenwasserstoffgemischen beliebigen aromatengehaltes

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DE59007835D1 (de) 1995-01-12
EP0418622A3 (en) 1992-11-04
DE3930992A1 (de) 1991-03-28
ES2064569T3 (es) 1995-02-01
EP0418622A2 (fr) 1991-03-27

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