EP0251838A1 - Process for the separation of solvent from a hydrocarbon solvent mixture and apparatus for performing this process - Google Patents

Process for the separation of solvent from a hydrocarbon solvent mixture and apparatus for performing this process Download PDF

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Publication number
EP0251838A1
EP0251838A1 EP87401232A EP87401232A EP0251838A1 EP 0251838 A1 EP0251838 A1 EP 0251838A1 EP 87401232 A EP87401232 A EP 87401232A EP 87401232 A EP87401232 A EP 87401232A EP 0251838 A1 EP0251838 A1 EP 0251838A1
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EP
European Patent Office
Prior art keywords
solvent
evaporation
installation
intermediate fluid
exchanger
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EP87401232A
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German (de)
French (fr)
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EP0251838B1 (en
Inventor
Patricia Delbourgo
Michel Coupard
Jean-Jacques Delorme
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Francaise dEtudes et de Construction Technip SA
Technip Energies France SAS
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Francaise dEtudes et de Construction Technip SA
Technip SA
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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
    • C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
    • C10G21/28—Recovery of used solvent
    • 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
    • Y10S203/02—Laboratory 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
    • Y10S203/04—Heat pump

Definitions

  • the present invention essentially relates to a process for the extraction of solvent from a mixture of solvent and of hydrocarbons without the addition of external heat.
  • the object of the present invention is to remedy the above drawbacks in particular by proposing a process and an installation for recovering solvent in solvent-hydrocarbon mixtures, which are particularly simple, reliable and inexpensive in the sense that they require no external heat supply.
  • the subject of the invention is a process for the separation of solvent from a mixture of solvent and of hydrocarbons, in which a stepwise evaporation of the solvent is carried out in order to separate it from the hydrocarbons, characterized in that the evaporation step of the solvent is carried out in a substantially isothermal manner in an order of decreasing pressures, and a heat exchange is carried out between the evaporated solvent and at least one intermediate fluid to obtain the condensation of the solvent and recover its heat of condensation so that said fluid intermediate, in the gas phase, can, after appropriate treatment, heat the mixture and carry out the evaporation of the solvent itself without an external heat supply to perform this operation is necessary.
  • the treatment of the aforementioned intermediate fluid in the gas phase consists in compressing this fluid to raise its temperature so as to allow the vaporization of the solvent.
  • the process of isothermal evaporation of the solvent is coupled with a heat pump which recovers the calories of condensation of the solvent and raises them to a sufficient thermal level so that they can be used for the clean solvent spray.
  • isothermal evaporation has high level energy saving advantages, which makes it possible to cover the calorie needs of this type with heat due to the irreversibility of the compression in the heat pump. .
  • the intermediate fluid recovering the heat of condensation of the solvent is water.
  • the temperature is preferably between 100 and 200 ° C.
  • the invention also relates to an installation for implementing the above process and of the type comprising at least two evaporation flasks or the like successively supplied by a charge consisting of a mixture to be separated, of solvent and of hydrocarbons, characterized by at least one steam generator ensuring the condensation of the solvent, by at least one circuit for transporting the evaporated solvent connecting the flasks to said generator, and by at least one intermediate fluid circuit in the gaseous phase comprising a means for raising the temperature condensing this fluid and connecting said generator to at least one exchanger disposed upstream of each tank.
  • the means for raising the condensation temperature of the intermediate fluid in the gas phase consists of at least one compressor.
  • an installation according to the invention comprises three successive flasks for evaporating the solvent and is characterized in that the streams of vaporized solvent leaving the second and the third flask are re-flow before reaching a first generator of vapet :, while the flow of vaporized solvent leaving the first balloon reaches a second steam generator, the condensed solvent streams leaving the two aforementioned generators being combined.
  • the flow of intermediate fluid in the gaseous phase produced by the two aforementioned generators feeds an exchanger upstream of the third balloon then divides to pass through two exchangers upstream of the first and second balloons respectively, and forms again a single flow passing through a heat exchanger for the charge introduced into the installation.
  • the installation shown in the single figure is, for example, the recovery section of solvent in dewaxed oil, of a dewaxing unit of lubricants.
  • the solvent used can be a mixture (50% -50% by volume) of methyl ethyl ketone and toluene.
  • the charge constituted by a solvent-oil mixture reaches the installation for example at a pressure of 500 kPa absolute and at a temperature of 39 ° C by a pipe to constitute flow 1.
  • the charge is divided into two flows marked respectively in 2 and 3, and it is preheated in an exchange train comprising, in parallel, the exchangers E 1 , E 2 and E 3 then the exchanger E4.
  • the stream 4 is heated by a stream of water vapor 111 to constitute the stream 6.
  • the stream 3 is heated by the dewaxed oil 23 going to storage via the pipe 24, and the stream 3 becomes the stream 5 which is joined to the stream 6 so as to form a single stream 7 reaching the 'exchanger E4.
  • the flow 7 is heated, up to the conditions of the evaporator or flash tank B l , by condensed water vapor 109.
  • the evaporator tank B 1 operates at a temperature of 148.5 ° C and at a pressure of 400 kPa absolute and makes it possible to vaporize approximately 40% of the solvent contained in the charge passing through line 8.
  • the mixed phase constituting the flow 10a after the valve V 1 and leading to the evaporator flask B 2 is heated in heat exchangers E 5 and E 6 to the aforementioned temperature of the evaporator flask B 2 .
  • the flow 10a is heated by the flow 9 of the vaporized solvent leaving the flask B 1 , and this heated flow 10a constitutes the flow 11 which is in turn heated by the exchanger E 6 thanks to the steam of condensed water passing through line 107.
  • the flash in the evaporator flask B 2 occurs, as said above, at a lower pressure than that of the flash in the flask B 1 , which makes it possible to eliminate practically all the remaining solvent which leaves the flask B 2 via the pipe 13.
  • the liquid leaving the flask B 2 is pumped into the bottom of this flask, passes through the pipe 14 and is heated by two exchangers in parallel E 7 and E 8 to a temperature of about 200 ° C which is the appropriate temperature for stripping hydrocarbons in a column C.
  • the derivative flow 14a is heated by the dewaxed oil leaving the column C via the line 22.
  • the derivative flow 14b is heated by the passing steam in a line 105 and produced by a steam compressor M.
  • This balloon operates at a temperature of 200 ° C and at a pressure of 243 kPa absolute identical to that of balloon B 2 .
  • the liquid fraction 21 leaving the flask B 3 is then stripped in the column C by water vapor 98 in order to remove the last traces of the solvent in the stream 99.
  • the dewaxed oil 22 leaving column C is, as explained above, sent to storage via line 24 after cooling in the exchangers E 8 and E 3 .
  • the vaporized solvent leaves the flask B 3 via line 20, and this vaporized solvent flow is mixed in 20a with the solvent flow 13 leaving the flask B 2 to constitute the solvent flow 25 (pressure 243 kPa absolute, temperature 154 ° C. ).
  • the vapors of stream 25 are completely condensed and then sub-cooled after passing through a first exchanger or steam generator G 1 carrying out the condensation of the solvent, and which is supplied with liquid water via a line 100.
  • the stream of solvent thus condensed forms the stream 26.
  • the stream of vaporized solvent 9 leaving the first evaporator flask B 1 is partially condensed in the exchanger E5 which arrives via line 27 at a second exchanger or steam generator G 29 which provides total condensation and the
  • the condensed solvent forms the flow 28, at the same temperature conditions as the flow 26.
  • the flow 28 is then expanded in a valve (not shown), then mixed with the flow 26, as seen in 28a, to form the flow 29 mentioned above which is cooled in the exchanger E l then sent to storage via a pipe 30.
  • the latter comprises for example two stages of compression and the steam is desuperheated between the two stages by water as shown by arrow 115.
  • the water vapor At the outlet of compressor M the water vapor is at around 220 ° C and 580 kPa absolute, and this water vapor passing through line 105 is used to supply high level calories to the exchanger E 7 upstream of the third ball B 3 .
  • the water vapor passes through the pipe 106 and divides to form the two pipes 107 and 109 passing through the exchangers E 6 and E 4 respectively to heat the supplies of the tanks B 2 and B 1 respectively.
  • the water vapor condensates then passing through the pipes 107a and 109a are mixed to form the stream 111 and are sub-cooled to 117 ° C and then expanded in a valve V 2 at a pressure of 180 kPa absolute, finally return to steam generators G 1 and G 2 via lines 100 and 102.
  • a process and an installation for recovering solvent have therefore been carried out according to the invention which have a much higher energy yield and which do not require external heat input, which heat supply serves in particular to compensate for the irreversibilities and the losses of the system.
  • the irreversibilities are minimized and the thermal degradation is reduced.
  • the heat between the process fluids and the heat pump fluid is transferred with minimal temperature degradation, which allows the system to work under optimal energy conditions.
  • the solvent is not heated to high temperatures during evaporation and will therefore undergo less thermal degradation.
  • the installation of the invention has remarkable operating stability by the fact that the heat recovered is mixed at the level of the heat pump and redistributed in parallel between the points of evaporation of the solvent, which allows d '' adjust the heat to be supplied to each flash separately.
  • the evaporation of the solvent in the flasks B 1 and B 2 is carried out in an order of decreasing pressures, so as to allow the evaporation of a very large amount of solvent while remaining at a substantially constant temperature, which may for example be between 100 and 200 ° C.
  • a substantially constant temperature which may for example be between 100 and 200 ° C.
  • the invention finally provides a method and an installation for recovering solvent which present exceptional results due to the fact that an isothermal evaporation scheme for the solvent is used, coupled with a heat pump recovering the calories of condensation of the solvent and raising them at a sufficient thermal level so that they can be used to ensure the proper vaporization of the solvent.
  • the method according to the invention can perfectly be incorporated into old solvent recovery installations.

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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)
  • Gas Separation By Absorption (AREA)

Abstract

La présente invention concerne un procédé et une installation de récupération de solvant à partir d'un mélange de solvant et d'hydrocarbures.The present invention relates to a process and an installation for recovering solvent from a mixture of solvent and hydrocarbons.

Cette installation comprend au moins deux ballons d'évaporation (B1, B2) successivement alimentés par une charge constituée par un mélange à séparer de solvant et d'hydrocarbures, au moins un générateur de vapeur effectuant la condensation du solvant (G1, G2), un circuit (27,13, 20) de transport du solvant évaporé reliant les ballons au générateur, et un circuit de fluide intermédiaire en phase gazeuse (104, 105, 106, 107, 109) comprenant un compresseur (M) pour élever la température de condensation de ce fluide, ce dernier circuit reliant le générateur à des échangeurs (E4, E6, E7) disposés en amont de chaque ballon (B1, B2, B3).This installation comprises at least two evaporation flasks (B 1 , B 2 ) successively supplied by a charge constituted by a mixture to be separated of solvent and of hydrocarbons, at least one steam generator carrying out the condensation of the solvent (G 1 , G 2 ), a circuit (27, 13, 20) for transporting the evaporated solvent connecting the flasks to the generator, and an intermediate fluid circuit in the gas phase (104, 105, 106, 107, 109) comprising a compressor (M) to raise the condensation temperature of this fluid, the latter circuit connecting the generator to exchangers (E 4 , E 6 , E 7 ) arranged upstream of each tank (B 1 , B 2 , B 3 ).

Une telle installation permet par example la récupération de solvant dans de l'huile déparaffinée.

Figure imgaf001
Such an installation allows for example the recovery of solvent in dewaxed oil.
Figure imgaf001

Description

La présente invention a essentiellement pour objet un procédé d'extraction de solvant d'un mélange de solvant et d'hydrocarbures sans apport de chaleur extérieure.The present invention essentially relates to a process for the extraction of solvent from a mixture of solvent and of hydrocarbons without the addition of external heat.

Elle vise également une installation pour la mise en oeuvre de ce procédé.It also relates to an installation for the implementation of this process.

On connait déjà un certain nombre de pro.cédés et d'installations d'extraction liquide-liquide au solvant où utilisant des solvants pour séparer des familles d'hydrocarbures. Mais ces procédés et installations sont très pénalisés, d'un point de vue du coût énergétique, par le fait qu'il faut séparer par la suite le solvant des phases d'extrait et de raffinat.We already know a certain number of processes and liquid-liquid solvent extraction installations where using solvents to separate families of hydrocarbons. However, these processes and installations are greatly penalized, from an energy cost point of view, by the fact that the solvent must subsequently be separated from the extract and raffinate phases.

Cette séparation ultime exige toujours un apport de chaleur extérieure au procédé ou à l'installation, cet apport se situant à un niveau thermique élevé, ce qui, comme on le comprend, augmente considérablement les coûts.This ultimate separation always requires a supply of heat outside the process or the installation, this supply being at a high thermal level, which, as it is understood, considerably increases the costs.

C'est ainsi que l'on connait des procédés consistant à recueillir les deux phases extrait-solvant et raffinat-solvant et à les chauffer dans un four ou par un fluide extérieur pour permettre l'évaporation du solvant et amener les hydrocarbures à une température adéquate afin d'obtenir une viscosité suffisamment faible permettant l'élimination par strippage des dernières traces de solvant.This is how processes are known which consist in collecting the two extract-solvent and raffinate-solvent phases and heating them in an oven or with an external fluid to allow the solvent to evaporate and bring the hydrocarbons to a temperature adequate in order to obtain a sufficiently low viscosity allowing elimination by stripping of the last traces of solvent.

On connait également des procédés plus performants qui réalisent des évaporations successives suivant un ordre de pressions croissantes. Dans ces procédés, le solvant est évaporé par un flash et est utilisé pour chauffer l'alimentation du flash précédent, de sorte qu'il est possible de réduire d'environ 30% l'apport de chaleur extérieure.There are also known more efficient processes which carry out successive evaporations according to an order of increasing pressures. In these methods, the solvent is evaporated by a flash and is used to heat the power supply of the previous flash, so that it is possible to reduce the external heat supply by about 30%.

Cependant, ces procédés présentent un certain nombre d'inconvénients.However, these methods have a number of drawbacks.

Ils exigent l'utilisation d'une source de chaleur extérieure (four ou huile chaude) qui est à une température très élevée, et ils sont d'une exploitation très instable puisque la moindre perturbation au niveau de la température ou du débit de la source chaude se répercute sur l'installation et la dérègle sévèrement. En outre, ces procédés et installations connus sont d'une mise en oeuvre complexe et exigent des empilages d'échangeurs et de colonnes nécessitant des structures encombrantes, coûteuses et se prêtant mal au remodelage des installations anciennes.They require the use of an external heat source (oven or hot oil) which is at a very high temperature, and they are of a very unstable operation since the least disturbance at the level of the temperature or the flow of the source heating affects the installation and severely disturbs it. In addition, these known methods and installations are of complex implementation and require stacking of exchangers and columns requiring bulky, costly structures and which do not lend themselves to remodeling of old installations.

La présente invention a pour but de remédier notamment aux inconvénients ci-dessus en proposant un procédé et une installation de récupération de solvant dans des mélanges solvant-hydrocarbures, qui sont particulièrement simples, fiables et peu coûteux en ce sens qu'ils ne nécessitent aucun apport de chaleur extérieure.The object of the present invention is to remedy the above drawbacks in particular by proposing a process and an installation for recovering solvent in solvent-hydrocarbon mixtures, which are particularly simple, reliable and inexpensive in the sense that they require no external heat supply.

A cet effet, l'invention a pour objet un procédé de séparation de solvant d'un mélange de solvant et d'hydrocarbures, dans lequel on effectue notamment une évaporation étagée du solvant pour le séparer des hydrocarbures, caractérisé en ce que l'évaporation étagée du solvant est effectuée de façon sensiblement isotherme en suivant un ordre de pressions décroissantes, et on effectue un échange de chaleur entre le solvant évaporé et au moins un fluide intermédiaire pour obtenir la condensation du solvant et récupérer sa chaleur de condensation afin que ledit fluide intermédiaire, en phase gazeuse, puisse, après traitement approprié, réchauffer le mélange et réaliser lui-même l'évaporation du solvant sans qu'un apport de chaleur extérieure pour effectuer cette opération soit nécessaire.To this end, the subject of the invention is a process for the separation of solvent from a mixture of solvent and of hydrocarbons, in which a stepwise evaporation of the solvent is carried out in order to separate it from the hydrocarbons, characterized in that the evaporation step of the solvent is carried out in a substantially isothermal manner in an order of decreasing pressures, and a heat exchange is carried out between the evaporated solvent and at least one intermediate fluid to obtain the condensation of the solvent and recover its heat of condensation so that said fluid intermediate, in the gas phase, can, after appropriate treatment, heat the mixture and carry out the evaporation of the solvent itself without an external heat supply to perform this operation is necessary.

On ajoutera ici que le traitement du fluide intermédiaire précité en phase gazeuse consiste à comprimer ce fluide pour élever sa température de façon à permettre la vaporisation du solvant.It will be added here that the treatment of the aforementioned intermediate fluid in the gas phase consists in compressing this fluid to raise its temperature so as to allow the vaporization of the solvent.

En d'autres termes, on comprend que le processus d'évaporation isotherme du solvant est couplé avec une pompe à chaleur qui récupère les calories de condensation du solvant et les remonte à un niveau thermique suffisant pour qu'elles puissent être utilisées pour la propre vaporisation du solvant. En outre, on comprend que l'évaporation isotherme présente des avantages d'économie en énergie de haut niveau, ce qui permet de couvrir les besoins en calories de ce type par la chaleur due à l'irréversibilité de la compression dans la pompe à chaleur. - Suivant une autre caractéristique du procédé de l'invention, le fluide intermédiaire récupérant la chaleur de condensation du solvant est de l'eau.In other words, it is understood that the process of isothermal evaporation of the solvent is coupled with a heat pump which recovers the calories of condensation of the solvent and raises them to a sufficient thermal level so that they can be used for the clean solvent spray. In addition, it is understood that isothermal evaporation has high level energy saving advantages, which makes it possible to cover the calorie needs of this type with heat due to the irreversibility of the compression in the heat pump. . - According to another characteristic of the process of the invention, the intermediate fluid recovering the heat of condensation of the solvent is water.

On précisera encore que, lors de l'évaporation étagée du solvant, la température est de préférence comprise entre 100 et 200°C.It will also be specified that, during the staged evaporation of the solvent, the temperature is preferably between 100 and 200 ° C.

L'invention vise également une installation pour la mise en oeuvre du procédé ci-dessus et du type comprenant au moins deux ballons ou analogues d'évaporation successivement alimentés par une charge constituée par un mélange à séparer, de solvant et d'hydrocarbures, caractérisée par au moins un générateur de vapeur assurant la condensation du solvant, par au moins un circuit de transport du solvant évaporé reliant les ballons audit générateur, et par au moins un circuit de fluide intermédiaire en phase gazeuse comprenant un moyen d'élévation de la température de condensation de ce fluide et reliant ledit générateur à au moins un échangeur disposé en amont de chaque ballon.The invention also relates to an installation for implementing the above process and of the type comprising at least two evaporation flasks or the like successively supplied by a charge consisting of a mixture to be separated, of solvent and of hydrocarbons, characterized by at least one steam generator ensuring the condensation of the solvent, by at least one circuit for transporting the evaporated solvent connecting the flasks to said generator, and by at least one intermediate fluid circuit in the gaseous phase comprising a means for raising the temperature condensing this fluid and connecting said generator to at least one exchanger disposed upstream of each tank.

On précisera ici que le moyen d'élévation de la température de condensation du fluide intermédiaire en phase gazeuse est constitué par au moins un compresseur.It will be specified here that the means for raising the condensation temperature of the intermediate fluid in the gas phase consists of at least one compressor.

Suivant un exemple de réalisation, une installation conforme à l'invention comprend trois ballons successifs d'évaporation du solvant et est caractérisée en ce que les flux de solvant vaporisa sortant du deuxième et du troisième ballon sont réuis avant de parvenir à un premier générateur de vapet:, tandis que le flux de solvant vaporisé sortant du premier ballon parvient à un deuxième générateur de vapeur, les flux de solvant condensés sortant des deux générateurs précités étant réunis.According to an exemplary embodiment, an installation according to the invention comprises three successive flasks for evaporating the solvent and is characterized in that the streams of vaporized solvent leaving the second and the third flask are re-flow before reaching a first generator of vapet :, while the flow of vaporized solvent leaving the first balloon reaches a second steam generator, the condensed solvent streams leaving the two aforementioned generators being combined.

Suivant encore une autre caractéristique de cette installation, le flux de fluide intermédiaire en phase gazeuse produit par les deux générateurs précités alimente un échangeur en amont du troisième ballon puis se divise pour traverser deux échangeurs en amont respectivement des premier et deuxième ballons, et forme à nouveau un flux unique traversant un échangeur de réchauffage de la charge introduite dans l'installation.According to yet another characteristic of this installation, the flow of intermediate fluid in the gaseous phase produced by the two aforementioned generators feeds an exchanger upstream of the third balloon then divides to pass through two exchangers upstream of the first and second balloons respectively, and forms again a single flow passing through a heat exchanger for the charge introduced into the installation.

On ajoutera ici que le flux unique précité est relié aux générateurs de vapeur.It will be added here that the aforementioned single flow is connected to the steam generators.

Mais d'autres caractéristiques et avantages de l'invention apparaîtront mieux dans la description détaillée qui suit et se réfère au dessin unique annexé, donné uniquement à titre d'exemple, et montrant d'une manière schématique une installation de récupération de solvant conforme aux principes de l'invention.However, other characteristics and advantages of the invention will appear better in the detailed description which follows and refers to the single appended drawing, given solely by way of example, and schematically showing a solvent recovery installation in accordance with principles of the invention.

L'installation représentée sur la figure unique, est par exemple, la section de récupération de.solvant dans l'huile déparaffinée, d'une unité de déparaffinage de lubrifiants.The installation shown in the single figure is, for example, the recovery section of solvent in dewaxed oil, of a dewaxing unit of lubricants.

Le solvant utilisé peut être un mélange (50%-50% en volume) de méthyléthylcétone et de toluène.The solvent used can be a mixture (50% -50% by volume) of methyl ethyl ketone and toluene.

La charge constituée par un mélange solvant-huile parvient à l'installation par exemple à une pression de 500 kPa absolus et à une température de 39°C par une conduite pour constituer le flux 1. La charge est divisée en deux flux repérés respectivement en 2 et 3, et elle est préchauffée dans un train d'échange comprenant, en parallèle, les échangeurs E1, E2 et E3 puis l'échangeur E4.The charge constituted by a solvent-oil mixture reaches the installation for example at a pressure of 500 kPa absolute and at a temperature of 39 ° C by a pipe to constitute flow 1. The charge is divided into two flows marked respectively in 2 and 3, and it is preheated in an exchange train comprising, in parallel, the exchangers E 1 , E 2 and E 3 then the exchanger E4.

Dans l'échangeur E1, la charge est réchauffée par le flux total de solvant condensé 29 et parvient à l'échangeur E2 par la conduite 4.In the exchanger E 1 , the charge is heated by the total flow of condensed solvent 29 and reaches the exchanger E 2 via the line 4.

Dans cet échangeur E2, le flux 4 est réchauffé par un flux de vapeur d'eau 111 pour constituer le flux 6.In this exchanger E 2 , the stream 4 is heated by a stream of water vapor 111 to constitute the stream 6.

Dans l'échangeur E3, le flux 3 est réchauffé par l'huile déparaffinée 23 allant au stockage par la conduite 24, et le flux 3 devient le flux 5 qui est réuni au flux 6 pour ainsi former un flux unique 7 parvenant à l'échangeur E4.In the exchanger E 3 , the stream 3 is heated by the dewaxed oil 23 going to storage via the pipe 24, and the stream 3 becomes the stream 5 which is joined to the stream 6 so as to form a single stream 7 reaching the 'exchanger E4.

Dans cet échangeur E4, le flux 7 est réchauffé, jusqu'aux conditions du ballon évaporateur ou de flash Bl, par de la vapeur d'eau condensée 109. Le ballon évaporateur B1 fonctionne à une température de 148,5°C et à une pression de 400 kPa absolus et permet de vaporiser environ 40% du solvant contenu dans la charge passant dans la conduite 8.In this exchanger E4, the flow 7 is heated, up to the conditions of the evaporator or flash tank B l , by condensed water vapor 109. The evaporator tank B 1 operates at a temperature of 148.5 ° C and at a pressure of 400 kPa absolute and makes it possible to vaporize approximately 40% of the solvent contained in the charge passing through line 8.

Le flux de solvant vaporisé sort du ballon B1 par la conduite 9, tandis que le liquide sortant de ce ballon par la conduite 10 est détendu dans une vanne V1 jusqu'à la-pression d'un deuxième ballon évaporatéur B2 qui fonctionne à une pression de 243 kPa, c'est-à-dire inférieure à la pression du ballon B1, et à une température de 150°C, c'est-à-dire sensiblement identique à celle du ballon B1. La phase mixte constituant le flux 10a après la vanne V1 et aboutissant au ballon évaporateur B2, est réchauffée dans des échangeurs de chaleur E5 et E6 jusqu'à la température précitée du ballon évaporateur B2.The flow of vaporized solvent leaves balloon B 1 via line 9, while the liquid leaving this balloon through line 10 is expanded in a valve V 1 until the pressure of a second evaporative balloon B 2 which operates at a pressure of 243 kPa, that is to say less than the pressure of the balloon B 1 , and at a temperature of 150 ° C., that is to say substantially identical to that of the balloon B 1 . The mixed phase constituting the flow 10a after the valve V 1 and leading to the evaporator flask B 2 , is heated in heat exchangers E 5 and E 6 to the aforementioned temperature of the evaporator flask B 2 .

Dans l'échangeur E5, le flux 10a est réchauffé par le flux 9 du solvant vaporisé sortant du ballon B1, et ce flux réchauffé 10a constitue le flux 11 qui est à son tour réchauffé par l'échangeur E6 grâce à la vapeur d'eau condensée passant dans la conduite 107.In the exchanger E 5 , the flow 10a is heated by the flow 9 of the vaporized solvent leaving the flask B 1 , and this heated flow 10a constitutes the flow 11 which is in turn heated by the exchanger E 6 thanks to the steam of condensed water passing through line 107.

Le flash dans le ballon évaporateur B2 se produit, comme dit précédemment, à une pression plus basse que celle du flash dans le ballon B1, ce qui permet d'éliminer pratiquement tout le solvant restant qui sort du ballon B2 par la conduite 13.The flash in the evaporator flask B 2 occurs, as said above, at a lower pressure than that of the flash in the flask B 1 , which makes it possible to eliminate practically all the remaining solvent which leaves the flask B 2 via the pipe 13.

Le liquide sortant du ballon B2 est pompé dans le fond de ce ballon, passe par la conduite 14 et est réchauffé par deux échangeurs en parallèle E7 et E8 jusqu'à une température d'environ 200°C qui est la température adéquate pour réaliser le strippage des hydrocarbures dans une colonne C.The liquid leaving the flask B 2 is pumped into the bottom of this flask, passes through the pipe 14 and is heated by two exchangers in parallel E 7 and E 8 to a temperature of about 200 ° C which is the appropriate temperature for stripping hydrocarbons in a column C.

Plus précisément, dans l'échangeur E8, le flux dérivé 14a est réchauffé par l'huile déparaffinée sortant de la colonne C par la conduite 22. Dans l'échangeur E7 le flux dérivé 14b est réchauffé par la vapeur d'eau passant dans une conduite 105 et produite par un compresseur de vapeur M.More precisely, in the exchanger E 8 , the derivative flow 14a is heated by the dewaxed oil leaving the column C via the line 22. In the exchanger E 7 the derivative flow 14b is heated by the passing steam in a line 105 and produced by a steam compressor M.

Après sortie des échangeurs E7 et E8, les deux flux dérivés 14a et 14b, qui sont à des températures différentes, sont remélangés pour constituer un flux 18 qui alimente un ballon B3.After leaving the exchangers E 7 and E 8 , the two derived flows 14a and 14b, which are at different temperatures, are remixed to form a flow 18 which feeds a balloon B 3 .

Ce ballon fonctionne à une température de 200°C et à une pression de 243 kPa absolus identique à celle du ballon B2.This balloon operates at a temperature of 200 ° C and at a pressure of 243 kPa absolute identical to that of balloon B 2 .

La fraction liquide 21 sortant du ballon B3 est alors strippée dans la colonne C par de la vapeur d'eau 98 afin d'éliminer les dernières traces du solvant dans le flux 99.The liquid fraction 21 leaving the flask B 3 is then stripped in the column C by water vapor 98 in order to remove the last traces of the solvent in the stream 99.

L'huile déparaffinée 22 sortant de la colonne C est, comme expliqué précédemment, envoyée au stockage par la conduite 24 après refroidissement dans les échangeurs E8 et E 3.The dewaxed oil 22 leaving column C is, as explained above, sent to storage via line 24 after cooling in the exchangers E 8 and E 3 .

Le solvant vaporisé sort du ballon B3 par la conduite 20, et ce flux de solvant vaporisé est mélangé en 20a au flux de solvant 13 sortant du ballon B2 pour constituer le flux de solvant 25 (pression 243 kPa absolus, température 154°C). Les vapeurs du flux 25 sont totalement condensées puis sous-refroidies après passage dans un premier échangeur ou générateur de vapeur G1 effectuant la condensation du solvant, et qui est alimenté en eau liquide par une conduite 100. Le flux de solvant ainsi condensé forme le flux 26.The vaporized solvent leaves the flask B 3 via line 20, and this vaporized solvent flow is mixed in 20a with the solvent flow 13 leaving the flask B 2 to constitute the solvent flow 25 (pressure 243 kPa absolute, temperature 154 ° C. ). The vapors of stream 25 are completely condensed and then sub-cooled after passing through a first exchanger or steam generator G 1 carrying out the condensation of the solvent, and which is supplied with liquid water via a line 100. The stream of solvent thus condensed forms the stream 26.

Le flux de solvant vaporisé 9 sortant du premier ballon évaporateur B1 est partiellement condensé dans l'échangeur E5 qui parvient par la conduite 27 à un deuxième échangeur ou générateur de vapeur G29 qui assure la condensation totale et leThe stream of vaporized solvent 9 leaving the first evaporator flask B 1 is partially condensed in the exchanger E5 which arrives via line 27 at a second exchanger or steam generator G 29 which provides total condensation and the

sous-refroidissement des vapeurs de solvant. Le solvant condensé forme le flux 28, aux mêmes conditions de température que le flux 26. Le flux 28 est alors détendu dans une vanne (non représentée), puis mélangé au flux 26, comme on le voit en 28a, pour former le flux 29 mentionné précédemment qui est refroidi dans l'échangeur El puis expédié au stockage par une conduite 30.solvent vapor subcooling. The condensed solvent forms the flow 28, at the same temperature conditions as the flow 26. The flow 28 is then expanded in a valve (not shown), then mixed with the flow 26, as seen in 28a, to form the flow 29 mentioned above which is cooled in the exchanger E l then sent to storage via a pipe 30.

On décrira maintenant le système formant pompe à chaleur constitué par les deux générateurs de vapeur G1, G2 alimentés en eau liquide par respectivement les conduites 100 et 102, par le compresseur M et par les échangeurs E2, E4, E6 et E7.We will now describe the system forming the heat pump consisting of the two steam generators G 1 , G 2 supplied with liquid water by the lines 100 and 102 respectively, by the compressor M and by the exchangers E 2 , E4, E 6 and E 7 .

La vapeur d'eau saturée produite par les deux générateurs de vapeur G1 et G2 et résultant de la récupération de la chaleur de condensation des flux de solvant 25 et 27, passe dans des conduits 101 et 103 qui sont réunis pour former un flux 104 de vapeur d'eau saturée, laquelle est comprimée par le compresseur M. Celui-ci comprend par exemple deux étages de compression et la vapeur est désurchauffée entre les deux étages par de l'eau comme matérialisé par la flèche 115.The saturated steam produced by the two steam generators G 1 and G 2 and resulting from the recovery of the heat of condensation of the solvent streams 25 and 27, passes through conduits 101 and 103 which are joined together to form a stream 104 of saturated steam, which is compressed by the compressor M. The latter comprises for example two stages of compression and the steam is desuperheated between the two stages by water as shown by arrow 115.

A la sortie du compresseur M la vapeur d'eau se trouve à environ 220°C et 580 kPa absolus, et cette vapeur d'eau passant par la conduite 105 est utilisée pour fournir des calories haut niveau à l'échangeur E7 en amont du troisième ballon B3. A la sortie de cet échangeur, la vapeur d'eau passe dans la conduite 106 et se divise pour former les deux conduites 107 et 109 traversant-respectivement les échangeurs E6 et E4 pour chauffer les alimentations des ballons B2 et B1 respectivement. Les condensats de vapeur d'eau passant ensuite dans les conduites 107a et 109a sont mélangés pour former le flux 111 et sont sous-refroidis jusqu'à 117°C puis détendus dans une vanne V2 à la pression de 180 kPa absolus, pour finalement retourner aux générateurs de vapeur G1 et G2 par les conduites 100 et 102.At the outlet of compressor M the water vapor is at around 220 ° C and 580 kPa absolute, and this water vapor passing through line 105 is used to supply high level calories to the exchanger E 7 upstream of the third ball B 3 . At the outlet of this exchanger, the water vapor passes through the pipe 106 and divides to form the two pipes 107 and 109 passing through the exchangers E 6 and E 4 respectively to heat the supplies of the tanks B 2 and B 1 respectively. The water vapor condensates then passing through the pipes 107a and 109a are mixed to form the stream 111 and are sub-cooled to 117 ° C and then expanded in a valve V 2 at a pressure of 180 kPa absolute, finally return to steam generators G 1 and G 2 via lines 100 and 102.

On se reportera maintenant au tableau ci-après pour constater les avantages de l'installation qui vient d'être décrite par rapport aux installations connues qui utilisent un apport de chaleur extérieure pour réaliser l'évaporation du solvant, alors que l'installation selon l'invention n'en utilise pas.

Figure imgb0001
Il apparaît immédiatement de ce tableau que le gain en énergie primaire représente environ 60% par rapport aux installations connues.We will now refer to the table below to see the advantages of the installation which has just been described compared to known installations which use an external heat supply to carry out the evaporation of the solvent, whereas the installation according to the the invention does not use it.
Figure imgb0001
 It immediately appears from this table that the gain in primary energy represents approximately 60% compared to known installations.

On a donc réalisé suivant l'invention un procédé et une installation de récupération de solvant qui présentent un rendement énergétique très supérieur et qui ne nécessitent pas d'apport extérieur de chaleur, lequel apport de chaleur sert notamment à compenser les irréversibilités et les pertes du système. Or, dans le schéma selon l'invention, les irréversibilités sont minimisées et la dégradation thermique est réduite. En d'autres termes, la chaleur entre les fluides procédé et le fluide de la pompe à chaleur est transférée avec une dégradation minimale de température, ce qui permet au système de travailler dans des conditions énergétiques optimales.A process and an installation for recovering solvent have therefore been carried out according to the invention which have a much higher energy yield and which do not require external heat input, which heat supply serves in particular to compensate for the irreversibilities and the losses of the system. However, in the scheme according to the invention, the irreversibilities are minimized and the thermal degradation is reduced. In other words, the heat between the process fluids and the heat pump fluid is transferred with minimal temperature degradation, which allows the system to work under optimal energy conditions.

On ajoutera encore que le solvant n'est pas chauffé à des températures élevées lors de l'évaporation et subira par conséquent une dégradation thermique moindre.It will also be added that the solvent is not heated to high temperatures during evaporation and will therefore undergo less thermal degradation.

On remarquera encore que l'installation de l'invention présente une stabilité de fonctionnement remarquable par le fait que la chaleur récupérée est mélangée au niveau de la pompe à chaleur et redistribuée en parallèle entre les points d'évaporation du solvant, ce qui permet d'ajuster séparément la chaleur à fournir à chaque flash.It will also be noted that the installation of the invention has remarkable operating stability by the fact that the heat recovered is mixed at the level of the heat pump and redistributed in parallel between the points of evaporation of the solvent, which allows d '' adjust the heat to be supplied to each flash separately.

Comme on l'a expliqué précédemment, l'évaporation du solvant dans les ballons B1 et B2 s'effectue suivant un ordre de pressions décroissantes, de façon à permettre l'évaporation d'une quantité très importante de solvant en restant à une température sensiblement constante et qui peut par exemple être comprise entre 100 et 200°C. Ceci permet encore une fois de minimiser les irréversibilités et d'avoir une demande de chaleur concentrée dans une plage très étroite de températures, ce qui convient parfaitement pour l'utilisation d'une pompe à chaleur.As explained previously, the evaporation of the solvent in the flasks B 1 and B 2 is carried out in an order of decreasing pressures, so as to allow the evaporation of a very large amount of solvent while remaining at a substantially constant temperature, which may for example be between 100 and 200 ° C. This again makes it possible to minimize the irreversibilities and to have a concentrated heat demand in a very narrow temperature range, which is perfectly suitable for the use of a heat pump.

L'invention procure finalement un procédé et une installation de récupération de solvant qui présentent des résultats exceptionnels dus au fait qu'on utilise un schéma d'évaporation isotherme du solvant couplé avec une pompe à chaleur récupérant les calories de condensation du solvant et les remontant à un niveau thermique suffisant pour qu'elles puissent être utilisées pour assurer la propre vaporisation du solvant.The invention finally provides a method and an installation for recovering solvent which present exceptional results due to the fact that an isothermal evaporation scheme for the solvent is used, coupled with a heat pump recovering the calories of condensation of the solvent and raising them at a sufficient thermal level so that they can be used to ensure the proper vaporization of the solvent.

Bien entendu, l'invention n'est nullement limitée au mode de réalisation décrit et illustré qui n'a été donné qu'à titre d'exemple.Of course, the invention is in no way limited to the embodiment described and illustrated, which has been given only by way of example.

C'est ainsi que le procédé selon l'invention peut parfaitement être incorporé dans les installations anciennes de récupération de solvant.Thus, the method according to the invention can perfectly be incorporated into old solvent recovery installations.

C'est dire que celle-ci comprend tous les équivalents techniques des moyens décrits ainsi que leurs combinaisons, si celles-ci sont effectuées suivant son esprit.This means that it includes all the technical equivalents of the means described as well as their combinations, if these are carried out according to the spirit.

Claims (9)

1. Procédé de séparation de solvant d'un mélange de solvant et d'hydrocarbures, dans lequel on effectue notamment une évaporation étagée du solvant pour le séparer des hydrocarbures, caractérisé en ce que l'évaporation étagée du solvant est effectuée de façon sensiblement isotherme en suivant un ordre de pressions décroissantes, et on effectue un échange de chaleur entre le solvant évaporé et au moins un fluide intermédiaire pour obtenir la condensation du solvant et récupérer sa chaleur de condensatin afin que ledit fluide intermédiaire, en phase gazeuse, puisse, après traitement approprié, réchauffer le mélange et réaliser lui-même l'évaporation du solvant sans qu'un apport de chaleur extérieure pour effectuer cette évaporation soit nécessaire.1. Process for the separation of solvent from a mixture of solvent and of hydrocarbons, in which a stepwise evaporation of the solvent is carried out in order to separate it from the hydrocarbons, characterized in that the stepwise evaporation of the solvent is carried out in a substantially isothermal manner following an order of decreasing pressures, and a heat exchange is carried out between the evaporated solvent and at least one intermediate fluid to obtain the condensation of the solvent and recover its condensate heat so that said intermediate fluid, in gaseous phase, can, after appropriate treatment, reheat the mixture and carry out the evaporation of the solvent itself without an external heat supply to effect this evaporation is necessary. 2. Procédé selon la revendication 1, caractérisé en ce que le traitement du fluide intermédiaire en phase gazeuse consiste à comprimer ce fluide pour élever sa température.2. Method according to claim 1, characterized in that the treatment of the intermediate fluid in the gas phase consists in compressing this fluid to raise its temperature. 3. Procédé selon la revendication 1 ou 2, caractérisé en ce que le fluide intermédiaire précité est de l'eau.3. Method according to claim 1 or 2, characterized in that the aforementioned intermediate fluid is water. 4. Procédé selon la revendication 1, caractérisé en ce que, lors de l'évaporation étagée précitée, la température est de préférence comprise entre 100 et 200°C.4. Method according to claim 1, characterized in that, during the aforementioned staged evaporation, the temperature is preferably between 100 and 200 ° C. 5. Installation pour la mise en oeuvre du procédé selon l'une des revendications 1 à 4, et du type comprenant au moins deux ballons ou analogues d'évaporation successivement alimentés par une charge constituée par un mélange à séparer de solvant et d'hydrocarbures, caractérisée par au moins un générateur de vapeur effectuant la condensation du solvant (G1, G2), par au moins un circuit (27, 13, 20 de transport du solvant évaporé reliant les ballons audit générateur, et par au moins un circuit de fluide intermédiaire en phase gazeuse (104, 105, 106, 107, 109) comprenant un moyen d'élévation de la température de condensation de ce fluide et reliant ledit générateur à au moins un échangeur (E4, E61 E7) disposé en amont de chaque ballon.5. Installation for the implementation of the method according to one of claims 1 to 4, and of the type comprising at least two flasks or the like of evaporation successively supplied by a charge consisting of a mixture to be separated from solvent and hydrocarbons , characterized by at least one steam generator carrying out the condensation of the solvent (G 1 , G 2 ), by at least one circuit (27, 13, 20 for transporting the evaporated solvent connecting the flasks to said generator, and by at least one circuit of intermediate fluid in the gas phase (104, 105, 106, 107, 109) comprising means for raising the condensation temperature of this fluid and connecting said generator to at least one exchanger ( E4, E61 E7 ) disposed upstream of each balloon. 6. Installation selon la revendication 5, caractérisé en ce que le moyen d'élévation de la température de condensation du fluide intermédiaire en phase gazeuse est constitué par au moins un compresseur (M).6. Installation according to claim 5, characterized in that the means for raising the condensation temperature of the intermediate fluid in the gas phase consists of at least one compressor (M). 7. Installation selon la revendication 5 ou 6, comprenant trois ballons successifs d'évaporation du solvant, caractérisée en ce que les flux de solvant vaporisés (13, 20) sortant du deuxième et du troisième ballons (B2, B3) sont réunis (20a) avant de parvenir à un premier générateur de vapeur (G1), tandis que le flux de solvant vaporisé (9) sortant du premier ballon (B1) parvient à un deuxième générateur de vapeur (G2), les flux de solvant condensé (26, 28) sortant des deux générateurs précités étant réunis.7. Installation according to claim 5 or 6, comprising three successive solvent evaporation flasks, characterized in that the streams of vaporized solvent (13, 20) leaving the second and third flasks (B 2 , B 3 ) are combined (20a) before reaching a first steam generator (G 1 ), while the flow of vaporized solvent (9) leaving the first balloon (B 1 ) reaches a second steam generator (G 2 ), the flows of condensed solvent (26, 28) leaving the two aforementioned generators being combined. 8. Installation selon l'une des revendications 5 à 7, caractérisée en ce que le flux de fluide intermédiaire en phase gazeuse (104) produit par les deux générateurs précités (G2, G2) alimente un échangeur (E7) en amont du troisième ballon (B3) puis se divise pour traverser deux échangeurs (E4, E6) en amont respectivement des premier (B1) et deuxième ballons (B2), et forme à nouveau un flux unique (111) traversant un échangeur (E2) de réchauffage de la charge (1) introduite dans l'installation.8. Installation according to one of claims 5 to 7, characterized in that the flow of intermediate fluid in the gas phase (104) produced by the two aforementioned generators (G 2 , G 2 ) feeds an exchanger (E 7 ) upstream of the third tank (B 3 ) then divides to pass through two exchangers (E4, E 6 ) upstream of the first (B 1 ) and second tanks respectively (B 2 ), and again forms a single flow (111) passing through an exchanger (E 2 ) for reheating the charge (1) introduced into the installation. 9. Installation selon l'une des revendications 5 à 8, caractérisée en ce que le flux unique précité (111) est relié aux générateurs de vapeur (G1, G2).9. Installation according to one of claims 5 to 8, characterized in that the aforementioned single flow (111) is connected to the steam generators (G 1 , G 2 ).
EP87401232A 1986-06-05 1987-06-02 Process for the separation of solvent from a hydrocarbon solvent mixture and apparatus for performing this process Expired EP0251838B1 (en)

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FR8608132 1986-06-05
FR8608132A FR2599750B1 (en) 1986-06-05 1986-06-05 METHOD FOR SEPARATING SOLVENT FROM A MIXTURE OF SOLVENT AND HYDROCARBONS, AND INSTALLATION COMPRISING APPLICATION OF THIS METHOD

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Citations (3)

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Publication number Priority date Publication date Assignee Title
US2276089A (en) * 1937-06-26 1942-03-10 Union Oil Co Recovery of solvents from oils
US4177137A (en) * 1977-11-07 1979-12-04 Standard Oil Company Aromatics extraction process
GB2084034A (en) * 1980-09-12 1982-04-07 Inst Francais Du Petrole Recovery of a light organic compound from a mixture with a heavy organic compound

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FR1543961A (en) * 1967-05-25 1968-10-31 Fives Lille Cail Installation for the production of fresh water from salt water
FR1562830A (en) * 1967-11-15 1969-04-11
US3607668A (en) * 1968-11-12 1971-09-21 Amf Inc Concentrated brine-incoming feed vapor compression desalination system
US4181577A (en) * 1974-07-18 1980-01-01 Auscoteng Pty. Ltd. Refrigeration type water desalinisation units
DE2600398C2 (en) * 1976-01-07 1985-01-10 Jakob Dr.-Ing. 8000 München Hoiß Process and device for raw water distillation
US4214975A (en) * 1978-05-10 1980-07-29 The Lummus Company Solvent recovery process for processing of hydrocarbons
US4390418A (en) * 1982-05-12 1983-06-28 Texaco Inc. Recovery of solvent in hydrocarbon processing systems

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Publication number Priority date Publication date Assignee Title
US2276089A (en) * 1937-06-26 1942-03-10 Union Oil Co Recovery of solvents from oils
US4177137A (en) * 1977-11-07 1979-12-04 Standard Oil Company Aromatics extraction process
GB2084034A (en) * 1980-09-12 1982-04-07 Inst Francais Du Petrole Recovery of a light organic compound from a mixture with a heavy organic compound

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US4830711A (en) 1989-05-16

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