EP0246956B1 - Process for the elimination of asphaltenes from a hydrocarbon feedstock - Google Patents

Process for the elimination of asphaltenes from a hydrocarbon feedstock Download PDF

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Publication number
EP0246956B1
EP0246956B1 EP87401091A EP87401091A EP0246956B1 EP 0246956 B1 EP0246956 B1 EP 0246956B1 EP 87401091 A EP87401091 A EP 87401091A EP 87401091 A EP87401091 A EP 87401091A EP 0246956 B1 EP0246956 B1 EP 0246956B1
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EP
European Patent Office
Prior art keywords
solvent
carbon atoms
hydrocarbon
fraction
volume
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EP87401091A
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German (de)
French (fr)
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EP0246956A1 (en
Inventor
Didier Chombart
François-Xavier Cormerais
Michel Laborde
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Total Marketing Services SA
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Total France SA
Compagnie de Raffinage et de Distribution Total France SA
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G21/00Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
    • C10G21/003Solvent de-asphalting
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G53/00Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
    • C10G53/02Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
    • C10G53/04Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step
    • C10G53/06Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step including only extraction steps, e.g. deasphalting by solvent treatment followed by extraction of aromatics

Definitions

  • the present invention relates to a process for deasphalting a heavy hydrocarbon feed.
  • heavy hydrocarbon filler is meant, within the meaning of the present invention, a filler having a density at 15 ° C greater than about 930 kg / m 3 , composed essentially of hydrocarbons, but also containing other chemical compounds which, in addition to carbon and hydrogen atoms, have heteroatoms such as oxygen, nitrogen, sulfur and metals such as vanadium or nickel.
  • This charge can be constituted, in particular, by a crude oil or a heavy oil having the density indicated above.
  • the feedstock can also come from the fractionation or processing of crude oil, heavy oil, oil shale or even coal. It may thus be the residue from the distillation under reduced pressure or the residue from the distillation at atmospheric pressure of the starting materials mentioned above or, for example, the products obtained by the heat treatment of these starting materials or their distillation residues.
  • the heaviest part of the heavy hydrocarbon charges consists of a mixture of an oily phase and an asphaltic phase.
  • One way to obtain light products from the oily phase is to subject it to catalytic cracking.
  • the catalytic cracking charge must not, however, be excessively polluted by metals and must not have an excessively high "Conradson” residue. It may be recalled that the "Conradson” residue, which gives indications on the tendency of a product to form coke, is determined according to the AFNOR NFT 60-116 standard.
  • heavy hydrocarbon feedstocks contain compounds having, in addition to hydrogen and carbon atoms, heteroatoms such as oxygen, nitrogen, sulfur and metals. Some of these compounds, especially those having metals, are contained in particular in the asphalt phase.
  • Asphaltenes like resins have polycyclic aromatic structures. Next to the aromatic rings are thiophenic and pyridine rings. But resins have less condensed structures than asphaltenes and lower molecular weights.
  • the compounds which precipitate by addition to the charge of a saturated aliphatic hydrocarbon having from 5 to 7 carbon atoms are generally designated under the name of asphaltenes: pentane, hexane, heptane.
  • pentane, hexane, heptane pentane, hexane, heptane.
  • a hydrocarbon with a lower boiling point for example propane.
  • this distinction is conventional and it is obvious that, if a given solvent is used at a given temperature to treat a charge, it will be possible, if the solvent and the temperature are suitable, to obtain the precipitation of asphaltene-type compounds . If the charge freed from asphaltenes is then treated with the same solvent at a higher temperature, precipitation of the resins can be obtained.
  • the deasphalting can be carried out in a single step, obtaining, in this case, an oily phase and an asphaltic phase, the latter containing both the asphaltenes and the resins. It can also be carried out in two stages, with the use of two different solvents and / or different operating conditions in the two stages (see, for example, US Pat . Nos . 3,830,732 and 2,940,920).
  • the oily phase, the resins and the asphaltenes are obtained separately, in this two-step process.
  • Also known from FR-A 2 007 587 is a process for deasphalting a heavy hydrocarbon feed, which uses two solvents in two stages.
  • the residual oil is separated into asphaltenes and into deasphaltenized oil using as solvent a hydrocarbon comprising from 5 to 10 carbon atoms.
  • the deasphalted oil is separated into resins and into deasphaltened oil and freed from the resins using as solvent one or more hydrocarbons, comprising less than 5 carbon atoms, for example propane, and mixtures thereof with aliphatic hydrocarbons comprising from 5 to 10 carbon atoms.
  • the asphaltenes fraction does not require an additional expense of flux to be used liquid.
  • the object of the present invention is therefore the preparation, in particular from a heavy hydrocarbon feedstock, of a product suitable as feedstock for a catalytic cracking.
  • the process is therefore characterized by a search for selectivity, which leads to the combination of two solvents containing little or no hydrocarbons with 4 carbon atoms, so as to vary the selectivity according to the stage at which one takes place. .
  • Solvents can consist of a single hydrocarbon, or a mixture of hydrocarbons; thus, the heavy solvent can consist of a mixture of pentane and hexane for example.
  • hydrocarbon pentane for example
  • it may be either a well-defined hydrocarbon, such as normal pentane, or also, and this is practically always the case industrially, of a mixture of isomers of this hydrocarbon, such as, in the case of pentane, normal pentane and isopentane, essentially.
  • the light solvent contains a higher proportion than the heavy hydrocarbon solvent comprising 3 carbon atoms.
  • the method according to the invention can be implemented in two different ways.
  • the first step is the step of separation of the "asphaltenes" fraction using the heavy solvent.
  • the "resins" fraction is then precipitated using a light solvent.
  • the treatment of the solution of the oily phase in the light solvent can in particular consist of heating said solution, preferably vaporizing the hydrocarbon comprising 3 carbon atoms.
  • the heating can be replaced by an expansion under reduced pressure of said solution.
  • the heavy solvent may preferably contain from 10 to 40% by volume of hydrocarbon with 3 carbon atoms and from 60 to 90% by volume d '' at least one hydrocarbon with at least 5 carbon atoms, and, better still, from 15 to 35% by volume of hydrocarbon with 3 carbon atoms and from 65 to 85% by volume of at least one hydrocarbon with at least 5 carbon atoms.
  • the light solvent may preferably contain from 20 to 80% by volume of hydrocarbon with 3 carbon atoms and from 20 to 80% by volume. volume of at least one hydrocarbon with at least 5 carbon atoms and, better still, from 25 to 75% by volume of hydrocarbon with 3 carbon atoms and from 25 to 75% by volume of at least one hydrocarbon with at minus 5 carbon atoms.
  • the light solvent may preferably contain from 20 to 80% by volume of hydrocarbon with 3 carbon atoms and from 20 to 80% by volume. volume of at least one hydrocarbon with at least 5 carbon atoms and, better still, from 30 to 70% by volume of at least one hydrocarbon with 3 carbon atoms and from 30 to 70% by volume of at least one hydrocarbon with at least 5 carbon atoms.
  • the heavy solvent may preferably contain from 5 to 30% by volume of hydrocarbon with 3 carbon atoms and from 70 to 95% by volume d '' at least one hydrocarbon with at least 5 carbon atoms and, better still, from 10 to 25% by volume of hydrocarbon with 3 carbon atoms and 75 to 90% by volume of at least one hydrocarbon with at least 5 atoms of carbon.
  • the hydrocarbon charge is introduced via line 1, into the upper part of a first extraction tower 2 heavy to deasphalt.
  • a heavy solvent the source of which will be explained later, is also introduced into the bottom of tower 2, via line 3.
  • the same heavy solvent can also be added to the feed in line 1, by a line not shown.
  • the heavy solvent of line 3 and the operating conditions of tower 2 are chosen so that only the "asphaltenes" fraction of feed 1 whose softening point is greater than or equal to 150 ° C. precipitates in said tower.
  • the pressure inside tower 2 can be between 20.105 and 1.10 7 absolute pascals, the temperature between 100 and 200 ° C, and the mass rate can be between 1 and 10, without these values being considered as limits.
  • the pressure may be approximately 40.10 5 absolute pascals, the temperatures at the bottom and at the top of tower 2 being respectively approximately 100 and 140 ° C., the mass ratio of heavy solvent on charge being approximately 2/1.
  • the "asphaltenes" fraction containing a little heavy solvent is collected at the bottom of tower 2, by line 4.
  • the charge is collected at the top of tower 2, via line 5, freed from the "asphaltenes" fraction, in solution in most of the heavy solvent introduced into tower 2.
  • the fraction collected by line 4 is conducted, after passing through at least one heater 6, in an expansion tower 7 operating, in the case of a heavy solvent C 3 -20 / C 5 -80, at a temperature of approximately 300 ° C and a pressure of approximately 5.105 absolute pascals. Heavy solvent is collected at the top of the tower 7, by the line 8, which, after passage through a coolant 9, is led into a flask 10.
  • the balloon 10 serves as storage for the heavy solvent.
  • the temperature in the flask 10 is approximately 60 ° C and the pressure approximately 5.10 5 absolute pascals.
  • the “asphaltenes” fraction is collected in the bottom of tower 7, by line 11, which is conducted in a tower 12, operating, in the case of a heavy solvent C 3 -20 / C 5 -80, at a temperature of about 300 ° C and a pressure of about 0.5.10 5 pascals absolute.
  • the “asphaltenes” fraction freed from the heavy solvent, is collected at the bottom of tower 12, via line 13. This fraction can be used as solid fuel after grinding.
  • Solvent is collected at the top of tower 12, via line 19, which is led into a condenser 14.
  • the mixture of heavy solvent and filler freed from the "asphaltenes" fraction collected by line 5 is carried out in a second extraction tower 20.
  • a third solvent is introduced into this tower, via line 21, so that , in tower 20, the extraction is carried out in fact using a light solvent, resulting from the combination of the heavy solvent and the third solvent and whose proportion of hydrocarbon with 3 carbon atoms is higher than that of the heavy solvent.
  • the third solvent can be a solvent C 3 -40 / C 5 -60, that is to say containing 40% by volume of propane and 60% by volume of pentane, the light solvent then being a solvent C 3 -30 / C 5 -70, containing 30% by volume of propane and 70% by volume of pentane.
  • the operating conditions inside tower 20 are such that the "resin" fraction precipitates.
  • the pressure inside tower 20 can be between 20.10 5 and 1.107 absolute pascals, the temperature between 100 and 300 ° C, the mass rate being between 1 and 10, without these values being considered as limits.
  • the pressure can be approximately 40 ⁇ 10 5 absolute pascals, the temperatures at the bottom and at the top of tower 20 being approximately, respectively, 110 and 150 ° C, the mass rate being about 4/1.
  • the "resins" fraction containing a little light solvent is collected at the bottom of tower 20, through line 28.
  • the mixture of deasphalted oily phase and of light solvent collected by line 22 is led, after passage through a heater 23, in an expansion tower 24 operating, in the case of a light solvent C 3 -30 / C 5 -70 , at a pressure of about 25.105 absolute pascals and a temperature of about 150 ° C.
  • a heater 23 As a result of the passage through the heater 23, part of the solvent is vaporized.
  • the hydrocarbon with 3 carbon atoms is preferably so.
  • a third solvent enriched in hydrocarbon with 3 carbon atoms is therefore collected at the top of tower 24, via line 25.
  • a third solvent C 3 -40 / C 5 -60 is thus obtained.
  • the third solvent collected by line 25 is led, after passage through a cooler 26, into a storage flask 27.
  • the temperature inside the tank 27 is around 110 ° C and the pressure around 25 bar.
  • the third solvent is then recycled via line 21 to tower 20.
  • the major part of the heavy solvent is collected at the top of the tower 32, via the line 33, which, after passing through a condenser 34, is led to the flask 10.
  • the flask 10 is connected by line 35 to line 3 and the heavy solvent can therefore be recycled to tower 2.
  • the deasphalted oily phase containing a small amount of solvent is collected at the bottom of the tower 32, via line 36, which, after passing through a heater 37, is conducted in a steam tower 38, where water vapor is introduced via line 39.
  • this tower operates at a pressure of approximately 1.5 ⁇ 10 5 absolute pascals and a temperature of approximately 250 ° C.
  • the deasphalted oil is collected at the bottom of the tower 38, by the line 41, and, at the top of the said tower, by the line 40, water and solvent, which are led to the condenser 14.
  • the "resins" fraction containing a little light solvent, collected by line 28 at the bottom of tower 20, is conducted, after passing through a heater 50, in an expansion tower 51 operating, in the case of a light solvent C 3 -30 / C 5 -70, at a pressure of approximately 5,105 absolute pascals and at a temperature of approximately 280 ° C.
  • the hydrocarbon charge is introduced via line 101, into the upper part of a first extraction tower 102 heavy to deasphalt.
  • a light solvent is also introduced into the bottom of tower 102, via line 103, the source of which will be explained below.
  • the "resins” and “asphaltenes” fractions precipitate.
  • the light solvent can be, for example, a solvent C 3 -60 / C s -40, containing 60% by volume of propane and 40% by volume of pentane.
  • the pressure inside tower 102 can be between 20.105 and 1.107 absolute pascals, the temperature between 100 and 300 ° C, the mass rate can be between 1 and 10, without these values being considered as limits.
  • the pressure may be approximately 40 ⁇ 10 5 absolute pascals, the temperatures at the bottom and at the top of the tower 102 being approximately, respectively, of 100 and 130 ° C, the mass rate
  • the solvent and the operating conditions of tower 109 are chosen so that only the "asphaltenes" fraction of line 105 whose softening point is greater than or equal to 150 ° C. precipitates in said tower.
  • the heavy solvent can be a solvent C 3 -20 / C 5 -80, the solvent of line 106 being a solvent C 3 -10 / C 5 -90.
  • the pressure inside tower 109 can be between 20.105 and 1.105 absolute pascals, the temperature between 100 and 200 ° C, the mass rate can be between 1 and 10, without these values being considered as limits.
  • the pressure can be around 40 ⁇ 10 5 absolute pascals, the temperatures at the bottom and at the top of the tower 109 being respectively about 100 and 140 ° C, the heavy solvent mass ratio on charge of tower 102 being approximately 2/1.
  • the "asphaltenes" fraction containing a little heavy solvent is collected at the bottom of tower 109, via line 110.
  • the mixture of "resins" fraction and of heavy solvent collected by line 111 is led, after passage through a heater 112, in an expansion tower 113 operating, in the case of a heavy solvent C 3 -20 / Cs-80 , at a pressure of approximately 25.10 5 absolute pascals and at a temperature of approximately 150 ° C. Following the passage through the heater 112, part of the solvent is vaporized.
  • the hydrocarbon with 3 carbon atoms is preferably so. Therefore, at the top of tower 113, by line 114, light solvent C 3 -60 / C 5 -40 is collected, which is recycled to line 103, after passage through a condenser 115, to reconstitute the solvent. slight drag in line 105.
  • the major part of the solvent is collected at the top of the tower 119, via the line 120, which, after passing through a condenser 121, is led to the flask 122.
  • the flask 122 is connected by line 123 to line 106 and the solvent can therefore be recycled.
  • this tower operates at a pressure of approximately 1.5 ⁇ 10 5 absolute pascals and a temperature of approximately 280 ° C.
  • the "resins” are collected at the bottom of the tower 126, by the line 128, and at the top of the said tower, by the line 129, water and solvent, which are led to the condenser 14 '.
  • a mixture of deasphalted oil and light solvent is collected at the top of the tower 102, via the line 129, which, after passing through a heater 131, is led into an expansion tower 132 operating, in the case of a light solvent C 3 -60 / C 5 -40, at a pressure of about 25,105 absolute pascals and a temperature of about 140 ° C.
  • the major part of the light solvent is collected at the top of tower 132, via line 133, which is recycled to line 103 through line 114 and the refrigerant 115.
  • the deasphalted oily phase containing a little solvent is collected at the bottom of tower 132, via line 134, which, after passing through a heater 135, is carried out in a tower 136 for driving with steam, where water vapor is introduced via line 137.
  • this tower operates at a pressure of approximately 1.5 ⁇ 10 5 absolute pascals and a temperature of approximately 250 ° C.
  • the deasphalted oil is collected at the bottom of the tower 136, by the line 138, and, at the top of the said tower, by the line 139, water and solvent, which are led to the condenser 14 '.
  • FIG. 3 represents a variant of FIG. 1, in which the separation of the light solvent from the deasphalted oil is carried out in such a way that the light solvent contains even more hydrocarbon with 3 carbon atoms.
  • the separation of the resins from the oil is better and allows an even "cleaner” deasphalted oil to be obtained, that is to say having an even lower “Conradson” residue.
  • the mixture of heavy solvent C 3 20 / C 5 -80 and of filler no longer containing "asphaltenes" collected by line 5 is led into a second extraction tower 200.
  • line 210 is introduced.
  • a third solvent C 3 -50 / C 5 -50 the extraction being carried out in fact using a light solvent C 3 -35 / C 5 -65.
  • the pressure in the tower can be approximately 40.10 s absolute pascals, the temperatures at the bottom and at the top of the tower 200 being approximately, respectively, 115 and 145 ° C., the mass rate being about 4/1.
  • the mixture of deasphalted oily phase and of light solvent C 5 -35 / C 5 -65 is collected at the top of the tower 200, via line 220.
  • the “resins” fraction containing a little light solvent is collected at the bottom of tower 200, by line 28, which is treated in the same way as for FIG. 1.
  • the mixture of deasphalted oily phase and light solvent C 3 -35 / C 5 -65 is led, after passage through a heater 230, in an expansion tower 240, operating, in the case of the light solvent C 3 -35 / C 5 -65, at a pressure of 25.10 s pascals absolute and a temperature of 145 ° C.
  • this phase after passing through a heater 370, is carried out in a water vapor drive tower 380, where water vapor is introduced via line 390.
  • deasphalted oil is collected by line 410 and, at the top of said tower, by line 400, water and solvent, which are led to condenser 14.
  • the process according to the invention is particularly useful, as the following examples show, for the simultaneous preparation of a deasphalted oil, suitable as a catalytic cracking charge, having a "Conradson" residue less than or equal to 10, preferably less than or equal to 9 and, better still, less than or equal to 8, and of an "asphaltenes" fraction, having a softening point equal to or greater than 150 ° C, preferably equal to or greater than 160 ° C and, better still, 170 ° C or higher.
  • This example relates to the treatment of a hydrocarbon feedstock constituted by the residue from the distillation under reduced pressure of the residue from the distillation under atmospheric pressure of a crude oil of Safaniya origin.
  • This charge is treated in a unit implementing the method according to the invention of the type presented in FIG. 1.
  • Solvents C 3 -C 5 are used in the unit, the compositions of which are given in Table 1 below.
  • This example relates to the treatment of a hydrocarbon feedstock constituted by the residue from the distillation under atmospheric pressure of the visbreaking effluent from a residue from the distillation under reduced pressure of a SAFANIYA crude oil.
  • This load is treated in a unit implementing the method according to the invention of the type shown in FIG. 1.
  • Solvents C 3 -C 5 are used in the unit with compositions identical to those of the solvents of Example 1.
  • This example relates to the treatment of a hydrocarbon feedstock constituted by the residue of the distillation under reduced pressure of the residue of the distillation under atmospheric pressure of a crude oil of Iraq origin.
  • This load is treated in a unit implementing the method according to the invention of the type shown in FIG. 1.
  • Solvents C 3 -C 6 are used in the unit, the compositions of which are given in Table VIII below. The operating conditions are given in Table IX below.
  • This example concerns the treatment of a hydrocarbon feedstock constituted by the residue from the distillation under reduced pressure of the residue from the distillation under atmospheric pressure of a crude oil of SAFANIYA origin.
  • This charge is treated in a unit implementing the method according to the invention of the type presented in FIG. 2.
  • Solvents C 3 -C 5 are used in the unit, the compositions of which are given in Table XII below. The operating conditions are given in Table XIII below.

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Description

La présente invention concerne un procédé de désasphaltage d'une charge hydrocarbonée lourde.The present invention relates to a process for deasphalting a heavy hydrocarbon feed.

Par charge hydrocarbonée lourde, on entend, au sens de la présente invention, une charge ayant une masse volumique à 15°C supérieure à environ 930 kg/m3, composée essentiellement d'hydrocarbures, mais contenant également d'autres composés chimiques qui, outre des atomes de carbone et d'hydrogène, possèdent des hétéroatomes, comme l'oxygène, l'azote, le soufre et des métaux comme le vanadium ou le nickel.By heavy hydrocarbon filler is meant, within the meaning of the present invention, a filler having a density at 15 ° C greater than about 930 kg / m 3 , composed essentially of hydrocarbons, but also containing other chemical compounds which, in addition to carbon and hydrogen atoms, have heteroatoms such as oxygen, nitrogen, sulfur and metals such as vanadium or nickel.

Cette charge peut être constituée, notamment, par un pétrole brut ou une huile lourde ayant la masse volumique indiquée ci-dessus.This charge can be constituted, in particular, by a crude oil or a heavy oil having the density indicated above.

La charge peut provenir également du fractionnement ou du traitement du pétrole brut, d'une huile lourde, de schistes bitumineux ou même de charbon. Il peut s'agir ainsi du résidu de la distillation sous pression réduite ou du résidu de la distillation sous pression atmosphérique des produits de départ cités ci-dessus ou, par exemple, des produits obtenus par le traitement thermique de ces produits de départ ou de leurs résidus de distillation.The feedstock can also come from the fractionation or processing of crude oil, heavy oil, oil shale or even coal. It may thus be the residue from the distillation under reduced pressure or the residue from the distillation at atmospheric pressure of the starting materials mentioned above or, for example, the products obtained by the heat treatment of these starting materials or their distillation residues.

Une tendance est apparue ces dernières années, de chercher à valoriser de plus en plus les produits hydrocarbonés ayant une masse volumique élevée, ce qui n'était pas le cas auparavant. Cette recherche de la valorisation des produits lourds est devenue plus pressante, car il est prévu que la demande de produits légers comme les carburants devrait augmenter relativement plus rapidement que celle des produits plus lourds, comme les fiouls.A trend has appeared in recent years, to seek to develop more and more hydrocarbon products with a high density, which was not the case before. This quest for the valuation of heavy products has become more pressing, since it is expected that the demand for light products such as fuels should increase relatively faster than that of heavier products, such as fuel oils.

La partie la plus lourde des charges hydrocarbonées lourdes est constituée d'un mélange d'une phase huileuse et d'une phase asphaltique. Un moyen d'obtenir des produits légers à partir de la phase huileuse est de soumettre celle-ci à un craquage catalytique. La charge de craquage catalytique ne doit toutefois pas être trop polluée par des métaux et ne pas présenter un résidu "Conradson" trop élevé. On peut rappeler que le résidu "Conradson", qui donne des indications sur la tendance d'un produit à former du coke, est déterminé selon la norme AFNOR NFT 60-116.The heaviest part of the heavy hydrocarbon charges consists of a mixture of an oily phase and an asphaltic phase. One way to obtain light products from the oily phase is to subject it to catalytic cracking. The catalytic cracking charge must not, however, be excessively polluted by metals and must not have an excessively high "Conradson" residue. It may be recalled that the "Conradson" residue, which gives indications on the tendency of a product to form coke, is determined according to the AFNOR NFT 60-116 standard.

Ainsi qu'il a été dit ci-dessus, les charges hydrocarbonées lourdes contiennent des composés possédant, outre des atomes d'hydrogène et de carbone, des hétéroatomes comme l'oxygène, l'azote, le soufre et des métaux. Certains de ces composés, notamment ceux possédant des métaux, sont contenus en particulier dans la phase asphaltique.As stated above, heavy hydrocarbon feedstocks contain compounds having, in addition to hydrogen and carbon atoms, heteroatoms such as oxygen, nitrogen, sulfur and metals. Some of these compounds, especially those having metals, are contained in particular in the asphalt phase.

On a l'habitude de distinguer deux familles dans les composés constituant la phase asphaltique: les résines et les asphaltènes. Les asphaltènes comme les résines ont des structures aromatiques polycycliques. A côté des cycles aromatiques se trouvent des cycles thiophéniques et pyridiniques. Mais les résines ont des structures moins condensées que les asphaltènes et des poids moléculaires plus faibles.We are used to distinguishing two families in the compounds constituting the asphalt phase: resins and asphaltenes. Asphaltenes like resins have polycyclic aromatic structures. Next to the aromatic rings are thiophenic and pyridine rings. But resins have less condensed structures than asphaltenes and lower molecular weights.

On désigne généralement sous le nom d'asphaltènes les composés qui précipitent par addition à la charge d'un hydrocarbure aliphatique saturé ayant de 5 à 7 atomes de carbone: pentane, hexane, heptane. Ainsi, selon la norme AFNOR NFT 60-115, la teneur en asphaltènes d'un produit est déterminée par une précipitation à l'aide du normal heptane à l'ébullition.The compounds which precipitate by addition to the charge of a saturated aliphatic hydrocarbon having from 5 to 7 carbon atoms are generally designated under the name of asphaltenes: pentane, hexane, heptane. Thus, according to AFNOR standard NFT 60-115, the asphaltene content of a product is determined by precipitation using normal heptane at boiling point.

Les résines précipitent en même temps que les asphaltènes, quand on utilise un hydrocarbure de plus faible point d'ébullition, par exemple le propane. En fait, cette distinction est conventionnelle et il est évident que, si on emploie, pour traiter une charge, un solvant donné à une température donnée, on pourra, si le solvant et la température sont appropriés, obtenir la précipitation de composés du type asphaltènes. Si on traite ensuite la charge débarrassée des asphaltènes par le même solvant à une température plus élevée, on pourra obtenir la précipitation des résines.Resins precipitate at the same time as asphaltenes, when using a hydrocarbon with a lower boiling point, for example propane. In fact, this distinction is conventional and it is obvious that, if a given solvent is used at a given temperature to treat a charge, it will be possible, if the solvent and the temperature are suitable, to obtain the precipitation of asphaltene-type compounds . If the charge freed from asphaltenes is then treated with the same solvent at a higher temperature, precipitation of the resins can be obtained.

Dans le procédé bien connu de désasphaltage, la phase huileuse et la phase asphaltique sont séparées par l'opération qui consiste à extraire du résidu la phase huileuse à l'aide d'un solvant. Ce solvant peut être choisi dans le groupe constitué par:

  • - les hydrocarbures aliphatiques, saturés ou non saturés, ayant de 2 à 8 atomes de carbone, seuls ou en mélange,
  • - les mélanges d'hydrocarbures, appelés distillats, ayant des poids moléculaires voisins de ceux des hydrocarbures ayant de 2 à 8 atomes de carbone,
  • - les mélanges de tous les hydrocarbures précédemment cités.
In the well-known deasphalting process, the oily phase and the asphaltic phase are separated by the operation which consists in extracting the oily phase from the residue using a solvent. This solvent can be chosen from the group consisting of:
  • - aliphatic hydrocarbons, saturated or unsaturated, having 2 to 8 carbon atoms, alone or as a mixture,
  • - mixtures of hydrocarbons, called distillates, having molecular weights close to those of hydrocarbons having from 2 to 8 carbon atoms,
  • - mixtures of all the previously mentioned hydrocarbons.

Le désasphaltage peut être effectué en une seule étape, avec obtention, dans ce cas, d'une phase huileuse et d'une phase asphaltique, cette dernière contenant à la fois les asphaltènes et les résines. Il peut également être effectué en deux étapes, avec utilisation de deux solvants différents et/ou des conditions opératoires différentes dans les deux étapes (voir, par exemple, les brevets US n° 3 830 732 et 2 940 920). On obtient de façon séparée, dans ce procédé en deux étapes, la phase huileuse, les résines et les asphaltènes.The deasphalting can be carried out in a single step, obtaining, in this case, an oily phase and an asphaltic phase, the latter containing both the asphaltenes and the resins. It can also be carried out in two stages, with the use of two different solvents and / or different operating conditions in the two stages (see, for example, US Pat . Nos . 3,830,732 and 2,940,920). The oily phase, the resins and the asphaltenes are obtained separately, in this two-step process.

Le brevet US N° 3 830 732 décrit ainsi un procédé utilisant deux solvants, le propane et le pentane, qui nécessite deux unités complètement séparées de récupération de solvant et, donc, un investissement important.US Patent No. 3,830,732 thus describes a process using two solvents, propane and pentane, which requires two completely separate solvent recovery units and, therefore, a significant investment.

Dans le procédé à un seul solvant (voir brevet US n° 2 940 920, par exemple), il est nécessaire et difficile d'ajuster très précisément les conditions opératoires des deux étapes pour obtenir les produits de qualités désirées. Il est même parfois impossible, avec ce procédé, d'obtenir à la fois une phase huileuse convenant comme charge de craquage catalytique et un brai très dur pouvant être broyé et être utilisé comme combustible solide.In the process with a single solvent (see US Patent No. 2,940,920, for example), it is necessary and difficult to very precisely adjust the operating conditions of the two stages in order to obtain the products of desired qualities. It is even sometimes impossible, with this process, to obtain both an oily phase suitable as a catalytic cracking charge and a very hard pitch which can be ground and used as solid fuel.

On connait aussi, par FR-A 2 007 587 un procédé de désasphaltage d'une charge hydrocarbonée lourde, qui utilise deux solvants en deux étapes. Dans la première étape, l'huile résiduelle est séparée en asphaltènes et en huile désasphalténisée utilisant comme solvant un hydrocarbure comprenant de 5 à 10 atomes de carbone. Dans la deuxième étape, l'huile désasphalténisée est séparée en résines et en huile désasphalténisée et débarrassée des résines en utilisant comme solvant un ou plusieurs hydrocarbures, comprenant moins de 5 atomes de carbone, par exemple le propane, et des mélanges de ceux-ci avec des hydrocarbures aliphatiques comprenant de 5 à 10 atomes de carbone.Also known from FR-A 2 007 587 is a process for deasphalting a heavy hydrocarbon feed, which uses two solvents in two stages. In the first stage, the residual oil is separated into asphaltenes and into deasphaltenized oil using as solvent a hydrocarbon comprising from 5 to 10 carbon atoms. In the second step, the deasphalted oil is separated into resins and into deasphaltened oil and freed from the resins using as solvent one or more hydrocarbons, comprising less than 5 carbon atoms, for example propane, and mixtures thereof with aliphatic hydrocarbons comprising from 5 to 10 carbon atoms.

La Demanderesse a conçu un procédé de désasphaltage en deux étapes, utilisant, lors des deux étapes, des solvants à la fois:

  • - relativement peu différents, ce qui permet de n'employer, au moins dans une forme de mise en oeuvre, qu'une seule installation de séparation de solvant,
  • - suffisamment différents, pour obtenir à la fois: une phase huileuse "propre" d'une qualité parfaitement convenable pour être utilisée comme charge de craquage catalytique, sans traitement complémentaire à l'hydrogène,
  • - et une fraction asphaltènes, qui, à température ambiante, est suffisamment solide pour être broyée et utilisée comme combustible solide.
The Applicant has designed a two-step deasphalting process, using, during the two steps, solvents at the same time:
  • - relatively little different, which makes it possible to use, at least in one form of implementation, only one solvent separation installation,
  • - sufficiently different, to obtain both: a "clean" oily phase of a quality perfectly suitable for use as a catalytic cracking charge, without additional treatment with hydrogen,
  • - And an asphaltenes fraction, which, at room temperature, is sufficiently solid to be ground and used as solid fuel.

De ce fait, la fraction asphaltènes ne nécessite pas une dépense supplémentaire de fluxant pour être utilisée liquide.Therefore, the asphaltenes fraction does not require an additional expense of flux to be used liquid.

Le but de la présente invention est donc la préparation, notamment à partir d'une charge hydrocarbonée lourde, d'un produit convenant comme charge d'un craquage catalytique.The object of the present invention is therefore the preparation, in particular from a heavy hydrocarbon feedstock, of a product suitable as feedstock for a catalytic cracking.

A cet effet, l'invention a pour objet un procédé de désasphaltage d'une charge hydrocarbonée lourde, ledit procédé conduisant à l'obtention:

  • - d'une phase huileuse désasphaltée ayant un indice "Conradson" égal ou inférieur à 10,
  • - d'une fraction "résines",
  • - d'une fraction "asphaltènes" ayant son point de ramollissement égal ou supérieur à 150°C, ledit procédé comportant deux étapes de précipitation, à partir de la charge, d'une part, de la fraction "asphaltènes" seule, d'autre part, de la fraction "résines", éventuellement en compagnie de la fraction "asphaltènes", à l'aide, respectivement, d'un solvant lourd et d'un solvant léger, ledit procédé étant caractérisé en ce que le solvant lourd contient de 5 à 40% en volume d'un hydrocarbure à 3 atomes de carbone et 60 à 95% d'au moins un hydrocarbure à 5 atomes de carbone et le solvant léger contient de 20 à 80% en volume d'un hydrocarbure à 3 atomes de carbone et de 20 à 80% en volume d'au moins un hydrocarbure à au moins 5 atomes de carbone, la proportion de l'hydrocarbure comprenant 3 atomes de carbone étant plus élevée dans le solvant léger que dans le solvant lourd.
To this end, the subject of the invention is a process for deasphalting a heavy hydrocarbon feed, said process leading to the obtaining:
  • - a deasphalted oily phase having a "Conradson" index equal to or less than 10,
  • - a "resin" fraction,
  • - an "asphaltenes" fraction having its softening point equal to or greater than 150 ° C., said process comprising two stages of precipitation, starting from the charge, on the one hand, of the "asphaltenes" fraction alone, on the other hand, from the "resins" fraction, optionally in the company of the "asphaltenes" fraction, using respectively a heavy solvent and a light solvent, said process being characterized in that the heavy solvent contains from 5 to 40% by volume of a hydrocarbon with 3 carbon atoms and 60 to 95% of at least one hydrocarbon with 5 carbon atoms and the light solvent contains from 20 to 80% by volume of a hydrocarbon with 3 carbon atoms and from 20 to 80% by volume of at least one hydrocarbon with at least 5 carbon atoms, the proportion of the hydrocarbon comprising 3 carbon atoms being higher in the light solvent than in the heavy solvent.

Dans cet objet de l'invention et dans la suite de la présente description, compte tenu du fait que la séparation au point de vue chimique entre la phase huileuse, les "résines" et les "asphaltènes", ne peut être définie de façon precise, on entend par:

  • 1. phase huileuse, une phase de. laquelle a été éliminée pratiquement toute la phase asphaltique, c'est-à-dire la phase qui précipite par addition d'un solvant léger tel que défini dans l'objet de l'invention; cette phase huileuse a un résidu "Conradson" inférieur ou égal à 10 (mesuré selon la norme AFNOR NFT 60-116);
  • 2. fraction "résines" et fraction "asphaltènes": les fractions respectivement la plus légère et la plus lourde de la phase asphaltique, la frontière entre ces deux fractions, au sens de l'invention, étant définie par le fait que la fraction "asphaltènes" doit avoir un point de ramollissement égal ou supérieur à 150°C (mesuré selon la norme AFNOR NFT 66-008).
In this object of the invention and in the remainder of this description, taking into account the fact that the separation from the chemical point of view between the oily phase, the "resins" and the "asphaltenes", cannot be precisely defined , we hear by:
  • 1. oily phase, a phase of. which has been eliminated practically all of the asphaltic phase, that is to say the phase which precipitates by adding a light solvent as defined in the subject of the invention; this oily phase has a "Conradson" residue less than or equal to 10 (measured according to standard AFNOR NFT 60-116);
  • 2. "resins" fraction and "asphaltenes" fraction: the lightest and heaviest fractions respectively of the asphaltic phase, the border between these two fractions, within the meaning of the invention, being defined by the fact that the fraction " asphaltenes "must have a softening point equal to or greater than 150 ° C (measured according to standard AFNOR NFT 66-008).

Dans le procédé selon l'invention, on utilise deux solvants, un solvant léger et un solvant lourd, qui contiennent les mêmes composés chimiques, mais dans des proportions différentes, ce qui explique leurs fonctions différentes:

  • - le solvant lourd est apte à faire précipiter la fraction "asphaltènes", mais solubilise la fraction "résines" et, a fortiori, la phase huileuse,
  • - le solvant léger est apte à faire précipiter la fraction "résines" et donc, bien sûr, la fraction "asphaltènes", mais solubilise la fraction huileuse.
In the process according to the invention, two solvents are used, a light solvent and a heavy solvent, which contain the same chemical compounds, but in different proportions, which explains their different functions:
  • the heavy solvent is capable of causing the "asphaltenes" fraction to precipitate, but dissolves the "resins" fraction and, a fortiori, the oily phase,
  • - The light solvent is able to precipitate the "resins" fraction and therefore, of course, the "asphaltenes" fraction, but dissolves the oily fraction.

Les deux solvants contiennent:

  • - au moins un hydrocarbure comprenant 3 atomes de carbone : propane et/ou propène,
  • - au moins un hydrocarbure comprenant au moins 5 atomes de carbone, aliphatique saturé ou oléfinique (dont, notamment, le pentane, le pentène, l'hexane, l'hexène, l'heptane, l'heptène).
The two solvents contain:
  • - at least one hydrocarbon comprising 3 carbon atoms: propane and / or propene,
  • - at least one hydrocarbon comprising at least 5 carbon atoms, saturated aliphatic or olefinic (including, in particular, pentane, pentene, hexane, hexene, heptane, heptene).

Le procédé est donc caractérisé par une recherche de sélectivité, qui conduit à la combinaison de deux solvants ne contenant que peu ou pas d'hydrocarbures à 4 atomes de carbone, de façon à faire varier la sélectivité suivant l'étape à laquelle on se place.The process is therefore characterized by a search for selectivity, which leads to the combination of two solvents containing little or no hydrocarbons with 4 carbon atoms, so as to vary the selectivity according to the stage at which one takes place. .

Les solvants peuvent être constitués d'un seul hydrocarbure, ou d'un mélange d'hydrocarbures; ainsi, le solvant lourd peut être constitué par un mélange de pentane et d'hexane par exemple.Solvents can consist of a single hydrocarbon, or a mixture of hydrocarbons; thus, the heavy solvent can consist of a mixture of pentane and hexane for example.

Il est entendu que, dans cette définition et dans la suite de la présente description, quand on cite un hydrocarbure, le pentane par exemple, il peut s'agir soit d'un hydrocarbure bien défini, tel que le normal pentane, soit également, et c'est industriellement pratiquement toujours le cas, d'un mélange d'isomères de cet hydrocarbure, tel que, dans le cas du pentane, le normal pentane et l'isopentane, essentiellement.It is understood that, in this definition and in the rest of the present description, when a hydrocarbon, pentane for example, is cited, it may be either a well-defined hydrocarbon, such as normal pentane, or also, and this is practically always the case industrially, of a mixture of isomers of this hydrocarbon, such as, in the case of pentane, normal pentane and isopentane, essentially.

Le solvant léger contient une proportion plus élevée que le solvant lourd d'hydrocarbure comprenant 3 atomes de carbone.The light solvent contains a higher proportion than the heavy hydrocarbon solvent comprising 3 carbon atoms.

Le procédé selon l'invention peut être mis en oeuvre de deux facons différentes.The method according to the invention can be implemented in two different ways.

Dans la première forme de mise en oeuvre du procédé selon l'invention, la première étape est l'étape de séparation de la fraction "asphaltènes" à l'aide du solvant lourd.In the first embodiment of the method according to the invention, the first step is the step of separation of the "asphaltenes" fraction using the heavy solvent.

On recueille, à l'issue de cette étape :

  • - d'une part, la fraction "asphaltènes" contenant un peu de solvant qui est éliminé ultérieurement,
  • - d'autre part, en solution dans le solvant lourd, la fraction "résines" et la phase huileuse.
At the end of this step, we collect:
  • on the one hand, the "asphaltenes" fraction containing a little solvent which is subsequently removed,
  • - on the other hand, in solution in the heavy solvent, the fraction "resins" and the oily phase.

La fraction "résines" est ensuite précipitée à l'aide d'un solvant léger.The "resins" fraction is then precipitated using a light solvent.

Pour obtenir ce solvant léger, dans une forme particulière de réalisation, on ajoute au mélange du solvant lourd, de la fraction résines et de la phase huileuse, dans une deuxième étape qui est l'étape de séparation des résines, un troisième solvant plus léger que le solvant léger, ce dernier résultant ainsi de la combinaison du solvant lourd et dudit troisième solvant. On recueille, à l'issue de cette étape :

  • - d'une part, la fraction résines contenant un peu de solvant, qui est éliminé ultérieurement,
  • - d'autre part, la phase huileuse en solution dans le solvant léger.
To obtain this light solvent, in a particular embodiment, a heavy solvent is added to the mixture of the heavy solvent, the resin fraction and the oily phase, in a second stage which is the stage of separation of the resins. as the light solvent, the latter thus resulting from the combination of the heavy solvent and said third solvent. At the end of this step, we collect:
  • on the one hand, the resin fraction containing a little solvent, which is subsequently removed,
  • - on the other hand, the oily phase in solution in the light solvent.

Cette solution est soumise ensuite à un traitement, qui permet d'obtenir:

  • - ledit troisième solvant, qui est recyclé à la deuxième étape,
  • - une solution de la phase huileuse dans le solvant lourd, dont elle est séparée de façon classique, le solvant lourd étant recyclé à la première étape.
This solution is then subjected to a treatment, which makes it possible to obtain:
  • - said third solvent, which is recycled in the second step,
  • - A solution of the oily phase in the heavy solvent, from which it is separated in a conventional manner, the heavy solvent being recycled in the first step.

Le traitement de la solution de la phase huileuse dans le solvant léger peut être notamment constitué par un chauffage de ladite solution vaporisant préférentiellement l'hydrocarbure comprenant 3 atomes de carbone.The treatment of the solution of the oily phase in the light solvent can in particular consist of heating said solution, preferably vaporizing the hydrocarbon comprising 3 carbon atoms.

Le chauffage peut être remplacé par une détente sous pression réduite de ladite solution.The heating can be replaced by an expansion under reduced pressure of said solution.

Dans la première étape de cette première forme de mise en oeuvre du procédé selon l'invention, le solvant lourd peut contenir de préférence de 10 à 40% en volume d'hydrocarbure à 3 atomes de carbone et de 60 à 90% en volume d'au moins un hydrocarbure à au moins 5 atomes de carbone, et, mieux encore, de 15 à 35 % en volume d'hydrocarbure à 3 atomes de carbone et de 65 à 85 % en volume d'au moins un hydrocarbure à au moins 5 atomes de carbone.In the first step of this first embodiment of the method according to the invention, the heavy solvent may preferably contain from 10 to 40% by volume of hydrocarbon with 3 carbon atoms and from 60 to 90% by volume d '' at least one hydrocarbon with at least 5 carbon atoms, and, better still, from 15 to 35% by volume of hydrocarbon with 3 carbon atoms and from 65 to 85% by volume of at least one hydrocarbon with at least 5 carbon atoms.

Dans la deuxième étape de cette première forme de mise en oeuvre du procédé selon l'invention, le solvant léger peut contenir, de préférence, de 20 à 80 % en volume d'hydrocarbure à 3 atomes de carbone et de 20 à 80 % en volume d'au moins un hydrocarbure à au moins 5 atomes de carbone et, mieux encore, de 25 à 75 % en volume d'hydrocarbure à 3 atomes de carbone et de 25 à 75 % en volume d'au moins un hydrocarbure à au moins 5 atomes de carbone.In the second step of this first embodiment of the process according to the invention, the light solvent may preferably contain from 20 to 80% by volume of hydrocarbon with 3 carbon atoms and from 20 to 80% by volume. volume of at least one hydrocarbon with at least 5 carbon atoms and, better still, from 25 to 75% by volume of hydrocarbon with 3 carbon atoms and from 25 to 75% by volume of at least one hydrocarbon with at minus 5 carbon atoms.

Dans la seconde forme de mise en oeuvre du procédé selon l'invention, la première étape est une étape de précipitation simultanée des fractions "résines" et "asphaltènes" à l'aide du solvant léger obtenu en combinant, lors de cette étape, le solvant lourd et un troisième solvant plus léger que le solvant léger désiré. On obtient, à l'issue de cette première étape :

  • - d'un part, un mélange des fractions "résines" et "asphaltènes",
  • - d'autre part, la phase huileuse en solution dans le solvant léger, dont elle est séparée ultérieurement.
In the second embodiment of the method according to the invention, the first step is a step of simultaneous precipitation of the "resin" and "asphaltene" fractions using the light solvent obtained by combining, during this step, the heavy solvent and a third solvent lighter than the desired light solvent. At the end of this first step, we obtain:
  • - on the one hand, a mixture of the "resins" and "asphaltenes" fractions,
  • - on the other hand, the oily phase in solution in the light solvent, from which it is separated later.

Dans une deuxième étape, on ajoute au mélange des fractions "résines" et "asphaltènes" du solvant lourd qui solubilise la fraction "résines". On obtient, à l'issue de cette seconde étape :

  • - d'une part, la fraction "asphaltènes" contenant un peu de solvant, qui est éliminé ultérieurement,
  • - d'autre part, la fraction "résines" en solution dans le solvant lourd, dont elle est séparée ultérieurement.
In a second step, "solvent" and "asphaltene" fractions are added to the mixture of heavy solvent which dissolves the "resin" fraction. At the end of this second step, we obtain:
  • - on the one hand, the "asphaltenes" fraction containing a little solvent, which is subsequently removed,
  • - on the other hand, the fraction "resins" in solution in the heavy solvent, from which it is separated later.

Dans la première étape de cette deuxième forme de mise en oeuvre du procédé selon l'invention, le solvant léger peut contenir, de préférence, de 20 à 80 % en volume d'hydrocarbure à 3 atomes de carbone et de 20 à 80 % en volume d'au moins un hydrocarbure à au moins 5 atomes de carbone et, mieux encore, de 30 à 70 % en volume d'au moins un hydrocarbure à 3 atomes de carbone et de 30 à 70 % en volume d'au moins un hydrocarbure à au moins 5 atomes de carbone.In the first step of this second embodiment of the process according to the invention, the light solvent may preferably contain from 20 to 80% by volume of hydrocarbon with 3 carbon atoms and from 20 to 80% by volume. volume of at least one hydrocarbon with at least 5 carbon atoms and, better still, from 30 to 70% by volume of at least one hydrocarbon with 3 carbon atoms and from 30 to 70% by volume of at least one hydrocarbon with at least 5 carbon atoms.

Dans la deuxième étape de cette deuxième forme de mise en oeuvre du procédé selon l'invention, le solvant lourd peut contenir de préférence de 5 à 30% en volume d'hydrocarbure à 3 atomes de carbone et de 70 à 95% en volume d'au moins un hydrocarbure à au moins 5 atomes de carbone et, mieux encore, de 10 à 25% en volume d'hydrocarbure à 3 atomes de carbone et 75 à 90% en volume d'au moins un hydrocarbure à au moins 5 atomes de carbone.In the second step of this second embodiment of the method according to the invention, the heavy solvent may preferably contain from 5 to 30% by volume of hydrocarbon with 3 carbon atoms and from 70 to 95% by volume d '' at least one hydrocarbon with at least 5 carbon atoms and, better still, from 10 to 25% by volume of hydrocarbon with 3 carbon atoms and 75 to 90% by volume of at least one hydrocarbon with at least 5 atoms of carbon.

Les conditions opératoires, dans les étages de désasphaltage, peuvent être les suivantes :

  • - pression comprise entre 20.105 et 1.107 pascals absolus,
  • - température comprise entre 100 et 300°C,
    Figure imgb0001
    entre 1 et 10.
The operating conditions, in the deasphalting stages, can be as follows:
  • - pressure between 20.10 5 and 1.10 7 absolute pascals,
  • - temperature between 100 and 300 ° C,
    Figure imgb0001
    between 1 and 10.

Ces conditions varient, bien sûr, notamment selon:

  • - la nature de la charge,
  • - la nature des solvants utilisés.
These conditions vary, of course, in particular according to:
  • - the nature of the load,
  • - the nature of the solvents used.

L'invention sera mieux comprise à la lecture de la description détaillée qui va suivre, en référence aux dessins annexés, qui n'ont pas de caractère limitatif.The invention will be better understood on reading the detailed description which follows, with reference to the accompanying drawings, which are not limiting.

Sur ces dessins:

  • Les figures 1 et 2 sont des schémas de deux unités mettant en oeuvre, respectivement, le premier mode et le second mode de réalisation du procédé selon l'invention.
  • La figure 3 illustre une variante de mise en oeuvre du procédé de la figure 1.
In these drawings:
  • Figures 1 and 2 are diagrams of two units implementing, respectively, the first mode and the second embodiment of the method according to the invention.
  • FIG. 3 illustrates an alternative implementation of the method of FIG. 1.

En référence à la figure 1, qui représente une unité mettant en oeuvre la première forme de réalisation du procédé selon l'invention, on introduit par la ligne 1, dans la partie supérieure d'une première tour d'extraction 2, la charge hydrocarbonée lourde à désasphalter. On introduit également dans le fond de la tour 2, par la ligne 3, un solvant lourd dont la provenance sera expliquée plus loin.With reference to FIG. 1, which represents a unit implementing the first embodiment of the method according to the invention, the hydrocarbon charge is introduced via line 1, into the upper part of a first extraction tower 2 heavy to deasphalt. A heavy solvent, the source of which will be explained later, is also introduced into the bottom of tower 2, via line 3.

Du même solvant lourd peut être également ajouté à la charge dans la ligne 1, par une ligne non représentée.The same heavy solvent can also be added to the feed in line 1, by a line not shown.

Le solvant lourd de la ligne 3 et les conditions opératoires de la tour 2 sont choisis de telle façon que seule la fraction "asphaltènes" de la charge 1 dont le point de ramollissement est supérieur ou égal à 150°C précipite dans ladite tour.The heavy solvent of line 3 and the operating conditions of tower 2 are chosen so that only the "asphaltenes" fraction of feed 1 whose softening point is greater than or equal to 150 ° C. precipitates in said tower.

La pression à l'intérieur de la tour 2 peut être comprise entre 20.105 et 1.107 pascals absolus, la température entre 100 et 200°C, et le taux massique

Figure imgb0002
peut être compris entre 1 et 10, sans que ces valeurs puissent être considérées comme des limites.The pressure inside tower 2 can be between 20.105 and 1.10 7 absolute pascals, the temperature between 100 and 200 ° C, and the mass rate
Figure imgb0002
can be between 1 and 10, without these values being considered as limits.

A titre d'exemple, pour un solvant lourd C3-20/C5-80, -c'est-à-dire contenant 20% en volume de propane et 80% en volume de pentane-, la pression peut être d'environ 40.105 pascals absolus, les températures en fond et en tête de la tour 2 étant respectivement d'environ 100 et 140°C, le taux massique solvant lourd sur charge étant d'environ 2/1.By way of example, for a heavy solvent C 3 -20 / C 5 -80, that is to say containing 20% by volume of propane and 80% by volume of pentane, the pressure may be approximately 40.10 5 absolute pascals, the temperatures at the bottom and at the top of tower 2 being respectively approximately 100 and 140 ° C., the mass ratio of heavy solvent on charge being approximately 2/1.

On recueille au fond de la tour 2, par la ligne 4, la fraction "asphaltènes" contenant un peu de solvant lourd.The "asphaltenes" fraction containing a little heavy solvent is collected at the bottom of tower 2, by line 4.

On recueille au sommet de la tour 2, par la ligne 5, la charge, débarrassée de la fraction "asphaltènes", en solution dans la majeure partie du solvant lourd introduit dans la tour 2.The charge is collected at the top of tower 2, via line 5, freed from the "asphaltenes" fraction, in solution in most of the heavy solvent introduced into tower 2.

La fraction recueillie par la ligne 4 est conduite, après passage dans au moins un réchauffeur 6, dans une tour de détente 7 fonctionnant, dans le cas d'un solvant lourd C3-20/C5-80, à une température d'environ 300°C et une pression d'environ 5.105 pascals absolus. On recueille au sommet de la tour 7, par la ¡'¡gne 8, du solvant lourd, qui est conduit, après passage dans un réfrigérant 9, dans un ballon 10.The fraction collected by line 4 is conducted, after passing through at least one heater 6, in an expansion tower 7 operating, in the case of a heavy solvent C 3 -20 / C 5 -80, at a temperature of approximately 300 ° C and a pressure of approximately 5.105 absolute pascals. Heavy solvent is collected at the top of the tower 7, by the line 8, which, after passage through a coolant 9, is led into a flask 10.

Le ballon 10 sert de stockage au solvant lourd. Dans le cas d'un solvant lourd C3-20/C5-80, la température dans le ballon 10 est d'environ 60°C et la pression d'environ 5.105 pascals absolus.The balloon 10 serves as storage for the heavy solvent. In the case of a heavy solvent C 3 -20 / C 5 -80, the temperature in the flask 10 is approximately 60 ° C and the pressure approximately 5.10 5 absolute pascals.

On recueille, dans le fond de la tour 7, par la ligne 11, la fraction "asphaltènes", qui est conduite dans une tour 12, fonctionnant, dans le cas d'un solvant lourd C3-20/C5-80, à une température d'environ 300°C et une pression d'environ 0,5.105 pascals absolus.The “asphaltenes” fraction is collected in the bottom of tower 7, by line 11, which is conducted in a tower 12, operating, in the case of a heavy solvent C 3 -20 / C 5 -80, at a temperature of about 300 ° C and a pressure of about 0.5.10 5 pascals absolute.

On recueille dans le fond de la tour 12, par la ligne 13, la fraction "asphaltènes" débarrassée du solvant lourd. Cette fraction peut être utilisée comme combustible solide après broyage.The “asphaltenes” fraction, freed from the heavy solvent, is collected at the bottom of tower 12, via line 13. This fraction can be used as solid fuel after grinding.

On recueille au sommet de la tour 12, par la ligne 19, du solvant qui est conduit dans un condenseur 14.Solvent is collected at the top of tower 12, via line 19, which is led into a condenser 14.

On recueille, à la sortie du condenseur 14 :

  • - par la ligne 15, de l'eau qui est évacuée (la provenance de cette eau est expliquée plus loin),
  • - et, dans le cas d'un solvant lourd C3-20/C5-80, par la ligne 16, le ou les hydrocarbures à au moins 5 atomes de carbone, qui est (ou sont) conduit(s) au ballon 10 et, par la ligne 17, l'hydrocarbure à 3 atomes de carbone qui, après passage dans un compresseur 18, est conduit dans la ligne 8 et donc au ballon 10.
We collect, at the outlet of the condenser 14:
  • - by line 15, water which is discharged (the source of this water is explained below),
  • - and, in the case of a heavy solvent C 3 -20 / C 5 -80, via line 16, the hydrocarbon (s) with at least 5 carbon atoms, which is (or are) conducted (s) in the balloon 10 and, via line 17, the hydrocarbon with 3 carbon atoms which, after passing through a compressor 18, is led into line 8 and therefore to balloon 10.

Le mélange du solvant lourd et de charge débarrassée de la fraction "asphaltènes" recueilli par la ligne 5 est conduit dans une deuxième tour d'extraction 20. On introduit dans cette tour, par la ligne 21, un troisième solvant, de telle façon que, dans la tour 20, l'extraction soit effectuée en fait à l'aide d'un solvant léger, résultant de la combinaison du solvant lourd et du troisième solvant et dont la proportion d'hydrocarbure à 3 atomes de carbone est plus élevée que celle du solvant lourd.The mixture of heavy solvent and filler freed from the "asphaltenes" fraction collected by line 5 is carried out in a second extraction tower 20. A third solvent is introduced into this tower, via line 21, so that , in tower 20, the extraction is carried out in fact using a light solvent, resulting from the combination of the heavy solvent and the third solvent and whose proportion of hydrocarbon with 3 carbon atoms is higher than that of the heavy solvent.

Ainsi, dans le cas d'un solvant lourd C3-20/C5-80, le troisième solvant peut être un solvant C3-40/C5-60, c'est-à-dire contenant 40 % en volume de propane et 60 % en volume de pentane, le solvant léger étant alors un solvant C3-30/C5-70, contenant 30 % en volume de propane et 70 % en volume de pentane.Thus, in the case of a heavy solvent C 3 -20 / C 5 -80, the third solvent can be a solvent C 3 -40 / C 5 -60, that is to say containing 40% by volume of propane and 60% by volume of pentane, the light solvent then being a solvent C 3 -30 / C 5 -70, containing 30% by volume of propane and 70% by volume of pentane.

Les conditions opératoires à l'intérieur de la tour 20 sont telles que la fraction "résines" précipite.The operating conditions inside tower 20 are such that the "resin" fraction precipitates.

La pression à l'intérieur de la tour 20 peut être comprise entre 20.105 et 1.107 pascals absolus, la température entre 100 et 300°C, le taux massique

Figure imgb0003
étant compris entre 1 et 10, sans que ces valeurs puissent être considérées comme limites.The pressure inside tower 20 can be between 20.10 5 and 1.107 absolute pascals, the temperature between 100 and 300 ° C, the mass rate
Figure imgb0003
being between 1 and 10, without these values being considered as limits.

A titre d'exemple, pour un solvant léger Ca-30/Cs-70, la pression peut être d'environ 40.105 pascals absolus, les températures en fond et en tête de la tour 20 étant environ, respectivement, de 110 et 150°C, le taux massique

Figure imgb0004
étant environ de 4/1.For example, for a light solvent Ca-30 / Cs-70, the pressure can be approximately 40 × 10 5 absolute pascals, the temperatures at the bottom and at the top of tower 20 being approximately, respectively, 110 and 150 ° C, the mass rate
Figure imgb0004
being about 4/1.

On recueille au sommet de la tour 20, par la ligne 22, un mélange de phase huileuse désasphaltée et de solvant léger.Is collected at the top of tower 20, through line 22, a mixture of deasphalted oily phase and light solvent.

On recueille au fond de la tour 20, par la ligne 28, la fraction "résines" contenant un peu de solvant léger.The "resins" fraction containing a little light solvent is collected at the bottom of tower 20, through line 28.

Le mélange de phase huileuse désasphaltée et de solvant léger recueilli par la ligne 22 est conduit, après passage dans un réchauffeur 23, dans une tour de détente 24 fonctionnant, dans le cas d'un solvant léger C3-30/C5-70, à une pression d'environ 25.105 pascals absolus et une tempéture d'environ 150°C. Par suite du passage dans le réchauffeur 23, une partie du solvant est vaporisée. L'hydrocarbure à 3 atomes de carbone l'est préférentiellement. On recueille de ce fait, au sommet de la tour 24, par la ligne 25, un troisième solvant enrichi en hydrocarbure à 3 atomes de carbone. Dans le cas d'un solvant léger C3-30/C5-70, on obtient ainsi un troisième solvant C3-40/C5-60.The mixture of deasphalted oily phase and of light solvent collected by line 22 is led, after passage through a heater 23, in an expansion tower 24 operating, in the case of a light solvent C 3 -30 / C 5 -70 , at a pressure of about 25.105 absolute pascals and a temperature of about 150 ° C. As a result of the passage through the heater 23, part of the solvent is vaporized. The hydrocarbon with 3 carbon atoms is preferably so. A third solvent enriched in hydrocarbon with 3 carbon atoms is therefore collected at the top of tower 24, via line 25. In the case of a light solvent C 3 -30 / C 5 -70, a third solvent C 3 -40 / C 5 -60 is thus obtained.

La mise en place de plateaux à l'intérieur de cette tour permet d'améliorer, si besoin est, la séparation.The installation of trays inside this tower improves, if necessary, the separation.

Le troisième solvant recueilli par la ligne 25 est conduit, après passage dans un réfrigérant 26, dans un ballon de stockage 27. Dans le cas d'un troisième solvant C3-40/C5-60, la température à l'intérieur du ballon 27 est d'environ 110°C et la pression d'environ 25 bars.The third solvent collected by line 25 is led, after passage through a cooler 26, into a storage flask 27. In the case of a third solvent C 3 -40 / C 5 -60, the temperature inside the tank 27 is around 110 ° C and the pressure around 25 bar.

Le troisième solvant est ensuite recyclé par la ligne 21 à la tour 20.The third solvent is then recycled via line 21 to tower 20.

On recueille au fond de la tour 24, par la ligne 29, un mélange d'huile désasphaltée et de solvant lourd, qui, après passage dans une vanne de détente 30, où sa pression et sa température sont abaissées (dans le cas d'un solvant lourd C3-20/Cs-80 à, respectivement, environ 5.105 pascals absolus et 100°C), et passage dans un réchauffeur 31, est conduit dans une tour de détente 32, fonctionnant, dans le cas d'un solvant lourd C3-20/C5-80, à une pression d'environ 5.105 pascals absolus et une température d'environ 130°C.Is collected at the bottom of the tower 24, through line 29, a mixture of deasphalted oil and heavy solvent, which, after passing through an expansion valve 30, where its pressure and temperature are lowered (in the case of a heavy solvent C 3 -20 / C s -80 at, respectively, about 5 × 10 5 absolute pascals and 100 ° C.), and passage through a heater 31, is led into an expansion tower 32, operating, in the case of a heavy solvent C 3 -20 / C 5 -80, at a pressure of approximately 5.10 5 absolute pascals and a temperature of approximately 130 ° C.

On recueille au sommet de la tour 32, par la ligne 33, la majeure partie du solvant lourd, qui, après passage dans un réfrigérant 34, est conduit au ballon 10.The major part of the heavy solvent is collected at the top of the tower 32, via the line 33, which, after passing through a condenser 34, is led to the flask 10.

Le ballon 10 est relié par la ligne 35 à la ligne 3 et le solvant lourd peut donc être recyclé à la tour 2.The flask 10 is connected by line 35 to line 3 and the heavy solvent can therefore be recycled to tower 2.

On recueille au fond de la tour 32, par la ligne 36, la phase huileuse désasphaltée contenant encore un peu de solvant qui, après passage dans un réchauffeur 37, est conduite dans une tour d'entraînement à la vapeur d'eau 38, où de la vapeur d'eau est introduite par la ligne 39.The deasphalted oily phase containing a small amount of solvent is collected at the bottom of the tower 32, via line 36, which, after passing through a heater 37, is conducted in a steam tower 38, where water vapor is introduced via line 39.

Dans le cas d'un solvant lourd C3-20/C5-80, cette tour fonctionne à une pression d'environ 1,5.105 pascals absolus et une température d'environ 250°C.In the case of a heavy solvent C 3 -20 / C 5 -80, this tower operates at a pressure of approximately 1.5 × 10 5 absolute pascals and a temperature of approximately 250 ° C.

On recueille au fond de la tour 38, par la ligne 41, l'huile désasphaltée et, au sommet de ladite tour, par la ligne 40, de l'eau et du solvant, qui sont conduits au condenseur 14.The deasphalted oil is collected at the bottom of the tower 38, by the line 41, and, at the top of the said tower, by the line 40, water and solvent, which are led to the condenser 14.

La fraction "résines" contenant un peu de solvant léger, recueillie par la ligne 28 au fond de la tour 20, est conduite, après passage dans un réchauffeur 50, dans une tour de détente 51 fonctionnant, dans le cas d'un solvant léger C3-30/C5-70, à une pression d'environ 5.105 pascals absolus et à une température d'environ 280°C.The "resins" fraction containing a little light solvent, collected by line 28 at the bottom of tower 20, is conducted, after passing through a heater 50, in an expansion tower 51 operating, in the case of a light solvent C 3 -30 / C 5 -70, at a pressure of approximately 5,105 absolute pascals and at a temperature of approximately 280 ° C.

On recueille, au sommet de la tour 51, par la ligne 52, un peu de solvant léger, qui est conduit à la ligne 8.A little light solvent is collected at the top of tower 51, via line 52, which is taken to line 8.

On recueille, au fond de la tour 51, par la ligne 53, la fraction "résines" contenant encore un peu de solvant, qui est conduite dans une tour d'entraînement à la vapeur d'eau 54, où de la vapeur d'eau est introduite par la ligne 55.Is collected at the bottom of tower 51, through line 53, the fraction "resins" still containing a little solvent, which is conducted in a steam tower 54, where steam water is introduced via line 55.

On recueille, au fond de la tour 54, par la ligne 57, la fraction "résines" qui peut être utilisée comme base fioul, être incorporée dans les bitumes, ou encore constituer une excellente charge de viscoréducteur.Is collected at the bottom of tower 54, through line 57, the fraction "resins" which can be used as an oil base, be incorporated into bitumens, or even constitute an excellent load of visbreaker.

On recueille au sommet de la tour 54, par la ligne 56, de l'eau et du solvant, qui sont conduits au condenseur 14.Water and solvent are collected at the top of the tower 54, via line 56, which are led to the condenser 14.

On peut noter que, si l'on introduit dans le ballon 10 du solvant lourd par la ligne 33, on introduit également du solvant léger provenant des lignes 52 et 56. Or, c'est le tout qui est recyclé comme solvant lourd. En fait, la quantité de solvant léger par rapport au solvant lourd est très faible et il suffit d'ajouter un peu d'hydrocarbure ayant au moins 5 atomes de carbone dans le ballon 10 pour obtenir un solvant lourd de composition correcte.It can be noted that, if heavy solvent is introduced into the flask 10 via line 33, light solvent is also introduced from lines 52 and 56. However, it is the whole which is recycled as heavy solvent. In fact, the quantity of light solvent relative to the heavy solvent is very small and it suffices to add a little hydrocarbon having at least 5 carbon atoms to the flask 10 to obtain a heavy solvent of correct composition.

Bien entendu, dans les unités représentées sur la figure 1, ainsi que sur les figures 2 et 3 qui vont être décrites ci-après, des appoints de solvants non représentés sont prévus pour compenser les pertes de solvant.Of course, in the units shown in FIG. 1, as well as in FIGS. 2 and 3 which will be described below, additions of solvents, not shown, are provided to compensate for the losses of solvent.

En référence à la figure 2, qui représente une unité mettant en oeuvre la deuxième forme de réalisation du procédé selon l'invention, on introduit par la ligne 101, dans la partie supérieure d'une première tour d'extraction 102, la charge hydrocarbonée lourde à désasphalter. On introduit également dans le fond de la tour 102, par la ligne 103, un solvant léger, dont la provenance sera expliquée plus loin. Les fractions "résines" et "asphaltènes" précipitent.With reference to FIG. 2, which represents a unit implementing the second embodiment of the method according to the invention, the hydrocarbon charge is introduced via line 101, into the upper part of a first extraction tower 102 heavy to deasphalt. A light solvent is also introduced into the bottom of tower 102, via line 103, the source of which will be explained below. The "resins" and "asphaltenes" fractions precipitate.

Le solvant léger peut être, par exemple, un solvant C3-60/Cs-40, contenant 60% en volume de propane et 40% en volume de pentane.The light solvent can be, for example, a solvent C 3 -60 / C s -40, containing 60% by volume of propane and 40% by volume of pentane.

La pression à l'intérieur de la tour 102 peut être comprise entre 20.105 et 1.107 pascals absolus, la température entre 100 et 300°C, le taux massique

Figure imgb0005
peut être compris entre 1 et 10, sans que ces valeurs puissent être considérées comme des limites.The pressure inside tower 102 can be between 20.105 and 1.107 absolute pascals, the temperature between 100 and 300 ° C, the mass rate
Figure imgb0005
can be between 1 and 10, without these values being considered as limits.

A titre d'exemple, pour un solvant léger C3-60/C5-40, la pression peut être d'environ 40.105 pascals absolus, les températures en fond et en tête de la tour 102 étant environ, respectivement, de 100 et 130°C, le taux massique

Figure imgb0006
For example, for a light solvent C 3 -60 / C 5 -40, the pressure may be approximately 40 × 10 5 absolute pascals, the temperatures at the bottom and at the top of the tower 102 being approximately, respectively, of 100 and 130 ° C, the mass rate
Figure imgb0006

étant environ de 2/1.being about 2/1.

On recueille, dans le fond de la tour 102, par la ligne 105, la totalité de la phase asphaltique contenant les fractions "asphaltènes" et "résines" et un peu de solvant léger. On ajoute à ce mélange, par la ligne 106, un solvant dont la provenance sera expliquée plus loin. Ce solvant contient peu d'hydrocarbures à 3 atomes de carbone. Ce nouveau mélange est conduit par la ligne 107, après passage dans un réchauffeur 108, dans une seconde tour d'extraction 109, où l'extraction est effectuée en présence d'un solvant lourd, grâce au mélange des solvants des lignes 105 et 106.The entire asphalt phase containing the "asphaltenes" and "resins" fractions and a little light solvent are collected at the bottom of tower 102, via line 105. To this mixture is added via line 106, a solvent whose source will be explained later. This solvent contains few hydrocarbons with 3 carbon atoms. This new mixture is conducted by line 107, after passing through a heater 108, in a second extraction tower 109, where the extraction is carried out in the presence of a heavy solvent, by mixing the solvents of lines 105 and 106 .

Le solvant et les conditions opératoires de la tour 109 sont choisis de telle façon que seule la fraction "asphaltènes" de la ligne 105 dont le point de ramollissement est supérieur ou égal à 150°C précipite dans ladite tour.The solvent and the operating conditions of tower 109 are chosen so that only the "asphaltenes" fraction of line 105 whose softening point is greater than or equal to 150 ° C. precipitates in said tower.

Si le solvant léger est un solvant C3-60/C5-40, le solvant lourd peut être un solvant C3-20/C5-80, le solvant de la ligne 106 étant un solvant C3-10/C5-90.If the light solvent is a solvent C 3 -60 / C 5 -40, the heavy solvent can be a solvent C 3 -20 / C 5 -80, the solvent of line 106 being a solvent C 3 -10 / C 5 -90.

La pression à l'intérieur de la tour 109 peut être comprise entre 20.105 et 1.105 pascals absolus, la température entre 100 et 200°C, le taux massique

Figure imgb0007
peut être compris entre 1 et 10, sans que ces valeurs puissent être considérées comme des limites.The pressure inside tower 109 can be between 20.105 and 1.105 absolute pascals, the temperature between 100 and 200 ° C, the mass rate
Figure imgb0007
can be between 1 and 10, without these values being considered as limits.

A titre d'exemple, pour un solvant lourd C3-20/C5-80, la pression peut être d'environ 40.10s pascals absolus, les températures en fond et en tête de la tour 109 étant respectivement d'environ 100 et 140°C, le taux massique solvant lourd sur charge de la tour 102 étant d'environ 2/1.For example, for a heavy solvent C 3 -20 / C 5 -80, the pressure can be around 40 × 10 5 absolute pascals, the temperatures at the bottom and at the top of the tower 109 being respectively about 100 and 140 ° C, the heavy solvent mass ratio on charge of tower 102 being approximately 2/1.

On recueille au fond de la tour 109, par la ligne 110, la fraction "asphaltènes" contenant un peu de solvant lourd.The "asphaltenes" fraction containing a little heavy solvent is collected at the bottom of tower 109, via line 110.

Le traitement de cette fraction est identique à celui de l'unité de la figure 1. Il ne sera pas décrit, dans un but de simplification. Cette partie de l'unité, identique à celle de la figure 1, à été représentée de la même façon, les numéros de référence des équipements étant affectés de l'indice '.The processing of this fraction is identical to that of the unit in FIG. 1. It will not be described, for the purpose of simplification. This part of the unit, identical to that of FIG. 1, has been represented in the same way, the reference numbers of the equipment being assigned the index '.

On recueille au sommet de la tour 109, par la ligne 111, un mélange de fraction "résines" et de solvant lourd.Is collected at the top of tower 109, by line 111, a mixture of fraction "resins" and heavy solvent.

Le mélange de fraction "résines" et de solvant lourd recueilli par la ligne 111 est conduit, après passage dans un réchauffeur 112, dans une tour de détente 113 fonctionnant, dans le cas d'un solvant lourd C3-20/Cs-80, à une pression d'environ 25.105 pascals absolus et à une température d'environ 150°C.Par suite du passage dans le réchauffeur 112, une partie du solvant est vaporisée. L'hydrocarbure à 3 atomes de carbone l'est préférentiellement. On recueille de ce fait, au sommet de la tour 113, par la ligne 114, du solvant léger C3-60/C5-40, qui est recyclé à la ligne 103, après passage dans un réfrigérant 115, pour reconstituer le solvant léger entraîné dans la ligne 105.The mixture of "resins" fraction and of heavy solvent collected by line 111 is led, after passage through a heater 112, in an expansion tower 113 operating, in the case of a heavy solvent C 3 -20 / Cs-80 , at a pressure of approximately 25.10 5 absolute pascals and at a temperature of approximately 150 ° C. Following the passage through the heater 112, part of the solvent is vaporized. The hydrocarbon with 3 carbon atoms is preferably so. Therefore, at the top of tower 113, by line 114, light solvent C 3 -60 / C 5 -40 is collected, which is recycled to line 103, after passage through a condenser 115, to reconstitute the solvent. slight drag in line 105.

La mise en place de plateaux à l'intérieur de cette tour 113 permet d'améliorer, si besoin est, la séparation.The establishment of trays inside this tower 113 improves, if necessary, the separation.

On recueille au fond de la tour 113, par la ligne 116, un mélange de "résines" et d'un solvant plus lourd que le solvant lourd, qui, après passage dans une vanne de détente 117, où sa pression et sa température sont abaissées, dans le cas d'un solvant C3-10/Cs-90, à respectivement environ 5.105 pascals absolus et 120°C, et passage dans un réchauffeur 118, est conduit dans une tour de détente 119, fonctionnant, dans le cas d'un solvant Cs-10/Cs-90, à une pression d'environ 5.105 pascals absolus et une température d'environ 140°C.Is collected at the bottom of tower 113, by line 116, a mixture of "resins" and a heavier solvent than the heavy solvent, which, after passing through an expansion valve 117, where its pressure and temperature are lowered, in the case of a solvent C 3 -10 / Cs-90, to respectively approximately 5,105 pascals absolute and 120 ° C, and passage through a heater 118, is conducted in a flash tower 119, operating, in the case of a solvent Cs-10 / Cs-90, at a pressure of approximately 5.105 absolute pascals and a temperature of approximately 140 ° C.

On receuille au sommet de la tour 119, par la ligne 120, la majeure partie du solvant, qui, après passage dans un réfrigérant 121, est conduit au ballon 122.The major part of the solvent is collected at the top of the tower 119, via the line 120, which, after passing through a condenser 121, is led to the flask 122.

Le ballon 122 est relié par la ligne 123 à la ligne 106 et le solvant peut donc être recyclé.The flask 122 is connected by line 123 to line 106 and the solvent can therefore be recycled.

On recueille au fond de la tour 119, par la ligne 124, la phase "résines" contenant encore un peu de solvant, qui, après passage dans un réchauffeur 125, est conduite dans une tour d'entraînement à la vapeur d'eau 126, où de la vapeur d'eau est introduite par la ligne 127.Is collected at the bottom of tower 119, through line 124, the phase "resins" still containing a little solvent, which, after passing through a heater 125, is conducted in a steam tower 126 , where water vapor is introduced via line 127.

Dans le cas d'un solvant C3-10/C5-90, cette tour fonctionne à une pression d'environ 1,5.105 pascals absolus et une température d'environ 280°C.In the case of a solvent C 3 -10 / C 5 -90, this tower operates at a pressure of approximately 1.5 × 10 5 absolute pascals and a temperature of approximately 280 ° C.

On recueille au fond de la tour 126, par la ligne 128, les "résines" et au sommet de ladite tour, par la ligne 129, de l'eau et du solvant, qui sont conduits au condenseur 14'.The "resins" are collected at the bottom of the tower 126, by the line 128, and at the top of the said tower, by the line 129, water and solvent, which are led to the condenser 14 '.

On recueille au sommet de la tour 102, par la ligne 129, un mélange d'huile désasphaltée et de solvant léger, qui, après passage dans un réchauffeur 131, est conduit dans une tour de détente 132 fonctionnant, dans le cas d'un solvant léger C3-60/C5-40, à une pression d'environ 25.105 pascals absolus et une température d'environ 140°C.A mixture of deasphalted oil and light solvent is collected at the top of the tower 102, via the line 129, which, after passing through a heater 131, is led into an expansion tower 132 operating, in the case of a light solvent C 3 -60 / C 5 -40, at a pressure of about 25,105 absolute pascals and a temperature of about 140 ° C.

On recueille au sommet de la tour 132, par la ligne 133, la majeure partie du solvant léger, qui est recyclé à la ligne 103 par la ligne 114 et le réfrigérant 115.The major part of the light solvent is collected at the top of tower 132, via line 133, which is recycled to line 103 through line 114 and the refrigerant 115.

On recueille au fond de la tour 132, par la ligne 134, la phase huileuse désasphaltée contenant encore un peu de solvant, qui, après passage dans un réchauffeur 135, est conduite dans une tour 136 d'entraînement à la vapeur d'eau, où de la vapeur d'eau est introduite par la ligne 137.The deasphalted oily phase containing a little solvent is collected at the bottom of tower 132, via line 134, which, after passing through a heater 135, is carried out in a tower 136 for driving with steam, where water vapor is introduced via line 137.

Dans le cas d'un solvant léger C3-60/C5-40, cette tour fonctionne à une pression d'environ 1,5.105 pascals absolus et une température d'environ 250°C.In the case of a light solvent C 3 -60 / C 5 -40, this tower operates at a pressure of approximately 1.5 × 10 5 absolute pascals and a temperature of approximately 250 ° C.

On recueille au fond de la tour 136, par la ligne 138, l'huile désasphaltée et, au sommet de ladite tour, par la ligne 139, de l'eau et du solvant, qui sont conduits au condenseur 14'.The deasphalted oil is collected at the bottom of the tower 136, by the line 138, and, at the top of the said tower, by the line 139, water and solvent, which are led to the condenser 14 '.

La figure 3 représente une variante de la figure 1, dans laquelle la séparation du solvant léger de l'huile désasphaltée est effectuée de telle façon que le solvant léger contienne encore plus d'hydrocarbure à 3 atomes de carbone. La séparation des résines de l'huile est meilleure et permet d'obtenir une huile désasphaltée encore plus "propre", c'est-à-dire ayant un résidu "Conradson" encore plus faible.FIG. 3 represents a variant of FIG. 1, in which the separation of the light solvent from the deasphalted oil is carried out in such a way that the light solvent contains even more hydrocarbon with 3 carbon atoms. The separation of the resins from the oil is better and allows an even "cleaner" deasphalted oil to be obtained, that is to say having an even lower "Conradson" residue.

Pour la description de cette figure, on prendra comme exemple un solvant lourd C3-20/C5-80 et un solvant léger C3-35/C5-65, mais, bien entendu, cet exemple de couple de solvants n'est pas limitatif.For the description of this figure, we will take as an example a heavy solvent C 3 -20 / C 5 -80 and a light solvent C 3 -35 / C 5 -65, but, of course, this example of a couple of solvents n ' is not limiting.

Seule la partie de la figure 3 différente de la figure 1 sera décrite et seuls les équipements contenant des produits différents ou différents eux-mêmes des équipements de la figure 1 ont été renumérotés, les autres organes conservent les mêmes chiffres de référence.Only the part of Figure 3 different from Figure 1 will be described and only the equipment containing different or different products themselves from the equipment of Figure 1 have been renumbered, the other bodies keep the same reference numbers.

Le mélange de solvant lourd C3 20/C5-80 et de charge ne contenant plus d"'asphaltènes" recueilli par la ligne 5 est conduit dans une deuxième tour d'extraction 200. On introduit dans cette tour, par la ligne 210, un troisième solvant C3-50/C5-50, l'extraction étant effectuée en fait à l'aide d'un solvant léger C3-35/C5-65. La pression dans la tour peut être d'environ 40.10s pascals absolus, les températures en fond et en tête de la tour 200 étant d'environ, respectivement, 115 et 145 °C, le taux massique

Figure imgb0008
étant d'environ de 4/1.The mixture of heavy solvent C 3 20 / C 5 -80 and of filler no longer containing "asphaltenes" collected by line 5 is led into a second extraction tower 200. In this tower, line 210 is introduced. , a third solvent C 3 -50 / C 5 -50, the extraction being carried out in fact using a light solvent C 3 -35 / C 5 -65. The pressure in the tower can be approximately 40.10 s absolute pascals, the temperatures at the bottom and at the top of the tower 200 being approximately, respectively, 115 and 145 ° C., the mass rate
Figure imgb0008
being about 4/1.

On recueille au sommet de la tour 200, par la ligne 220, le mélange de phase huileuse désasphaltée et de solvant léger C5-35/C5-65.The mixture of deasphalted oily phase and of light solvent C 5 -35 / C 5 -65 is collected at the top of the tower 200, via line 220.

On recueille au fond de la tour 200, par la ligne 28, la fraction "résines" contenant un peu de solvant léger, qui est traitée de la même façon que pour la figure 1. Le mélange de phase huileuse désasphaltée et de solvant léger C3-35/C5-65 est conduit, après passage dans un réchauffeur 230, dans une tour de détente 240, fonctionnant, dans le cas du solvant léger C3-35/C5-65, à une pression de 25.10s pascals absolus et une température de 145°C.The “resins” fraction containing a little light solvent is collected at the bottom of tower 200, by line 28, which is treated in the same way as for FIG. 1. The mixture of deasphalted oily phase and light solvent C 3 -35 / C 5 -65 is led, after passage through a heater 230, in an expansion tower 240, operating, in the case of the light solvent C 3 -35 / C 5 -65, at a pressure of 25.10 s pascals absolute and a temperature of 145 ° C.

La tour 240 est équipée de trois soutirages. Par suite de la vaporisation partielle de l'hydrocarbure à 3 atomes de carbone, on recueille:

  • - au fond de la tour, par la ligne 290, un mélange d'huile désasphaltée et de solvant C3-20/C5-80, qui, après passage dans une vanne de détente 300, où sa pression et sa température sont abaissées, respectivement, à 5.105 pascals absolus et 95°C, et passage dans un réchauffeur 310, est conduit dans une tour de détente 320 fonctionnant à une pression de 5.10s pascals absolus et une température d'environ 120°C,
  • - par un soutirage latéral 500, un solvant C3-30/C5-70, dont une partie est conduite à la ligne 33, l'autre partie étant recyclée à la tour 240 par la ligne 510, après passage dans un réfrigérant 520;
  • - au sommet de la tour 240, par la ligne 250, un solvant C3-50/C550, qui, après passage dans un réfrigérant 260, est conduit dans un ballon de stockage 270, ce solvant étant ensuite recyclé à la tour 200 par la ligne 210.
Tower 240 is equipped with three rackings. As a result of the partial vaporization of the hydrocarbon with 3 carbon atoms, we collect:
  • - at the bottom of the tower, via line 290, a mixture of deasphalted oil and solvent C 3 -20 / C 5 -80, which, after passing through an expansion valve 300, where its pressure and temperature are lowered , respectively, at 5.105 absolute pascals and 95 ° C, and passage through a heater 310, is conducted in an expansion tower 320 operating at a pressure of 5.10 s absolute pascals and a temperature of approximately 120 ° C,
  • - by a lateral racking 500, a solvent C 3 -30 / C 5 -70, part of which is taken to line 33, the other part being recycled to tower 240 by line 510, after passing through a refrigerant 520 ;
  • - at the top of tower 240, via line 250, a solvent C 3 -50 / C 5 50, which, after passing through a refrigerant 260, is led into a storage flask 270, this solvent then being recycled to the tower 200 by line 210.

La tour 320 est équipée de trois soutirages:

  • - au sommet de cette tour, on recueille, par la ligne 528, du solvant C3-50/C5-50, qui est recyclé à la ligne 250;
  • - on recueille, par un soutirage latéral 530, un solvant C3-15/C5-85 dont une partie est conduite à la ligne 33, tandis que l'autre partie est recyclée dans la tour 320, par la ligne 550, après passage dans un réfrigérant 540;
  • - on recueille, au fond de la tour 320, par la ligne 360, la phase huileuse désasphaltée contenant un peu de solvant.
Tower 320 is equipped with three withdrawals:
  • - At the top of this tower, there is collected, via line 528, solvent C 3 -50 / C 5 -50, which is recycled to line 250;
  • - A solvent C 3 -15 / C 5 -85 is collected by a lateral withdrawal 530, part of which is taken to line 33, while the other part is recycled in tower 320, by line 550, after passage through a refrigerant 540;
  • - The deasphalted oily phase containing a little solvent is collected at the bottom of tower 320, via line 360.

Comme dans le cas de la figure 1, en vue d'éliminer le solvant de la phase huileuse, de la ligne 360, cette phase, après passage dans un réchauffeur 370, est conduite dans une tour d'entraînement à la vapeur d'eau 380, où de la vapeur d'eau est introduite par la ligne 390.As in the case of FIG. 1, with a view to removing the solvent from the oily phase, from line 360, this phase, after passing through a heater 370, is carried out in a water vapor drive tower 380, where water vapor is introduced via line 390.

Au fond de la tour 380, on recueille, par la ligne 410, l'huile désasphaltée et, au sommet de ladite tour, par la ligne 400, de l'eau et du solvant, qui sont conduits au condenseur 14.At the bottom of tower 380, deasphalted oil is collected by line 410 and, at the top of said tower, by line 400, water and solvent, which are led to condenser 14.

La combinaison des solvants des lignes 500 et 530 permet d'obtenir un solvant lourd C3-20/C5-80, qui est recyclé à partir du ballon 10 à la ligne 3.The combination of the solvents of lines 500 and 530 makes it possible to obtain a heavy solvent C 3 -20 / C 5 -80, which is recycled from the flask 10 to line 3.

On voit, à cette description de la figure 3, que, grâce aux deux soutirages latéraux des tours 240 et 320, il est possible d'enrichir le solvant léger en hydrocarbure à 3 atomes de carbone.It can be seen from this description of FIG. 3 that, thanks to the two lateral withdrawals from towers 240 and 320, it is possible to enrich the light solvent with a hydrocarbon with 3 carbon atoms.

Le procédé selon l'invention est particulièrement utile, comme le montrent les exemples suivants, pour la préparation simultanée d'une huile désasphaltée, convenant comme charge de craquage catalytique, ayant un résidu "Conradson" inférieur ou égal à 10, de préférence inférieur ou égal à 9 et, mieux encore, inférieur ou égal à 8, et d'une fraction "asphaltènes", ayant un point de ramollissement égal ou supérieur à 150°C, de préférence égal ou supérieur à 160°C et, mieux encore, égal ou supérieur à 170°C.The process according to the invention is particularly useful, as the following examples show, for the simultaneous preparation of a deasphalted oil, suitable as a catalytic cracking charge, having a "Conradson" residue less than or equal to 10, preferably less than or equal to 9 and, better still, less than or equal to 8, and of an "asphaltenes" fraction, having a softening point equal to or greater than 150 ° C, preferably equal to or greater than 160 ° C and, better still, 170 ° C or higher.

Ces exemples sont destinés à illustrer l'invention de façon non limitative.These examples are intended to illustrate the invention without limitation.

EXEMPLE 1EXAMPLE 1

Cet exemple concerne le traitement d'une charge hydrocarbonée constituée par le résidu de la distillation sous pression réduite du résidu de la distillation sous pression atmosphérique d'un pétrole brut d'origine Safaniya.This example relates to the treatment of a hydrocarbon feedstock constituted by the residue from the distillation under reduced pressure of the residue from the distillation under atmospheric pressure of a crude oil of Safaniya origin.

Les caractéristiques de cette charge sont les suivantes :

  • - masse volumique à 15°C (measurée selon la norme AFNOR NFT 60-101): 1035 kg/m3,
  • - viscosité à 100°C (mesurée selon la norme AFNOR NFT 60-100) : 0,56.10-2 m2/s,
  • - résidu "Conradson" (mesuré selon la norme AFNOR NFT 60-116) : 23 % en poids,
  • - teneur en :
  • * asphaltènes (mesurée selon la norme AFNOR NFT 60-115) : 16 % en poids,
  • * soufre (mesurée par fluorescence -X) : 5,5% en poids,
  • * nickel (mesurée par fluorescence X) : 43 p.p.m.,
  • * vanadium (mesurée par fluorescence X): 138 p.p.m.
The characteristics of this charge are as follows:
  • - density at 15 ° C (measured according to AFNOR NFT 60-101 standard): 1035 kg / m 3 ,
  • - viscosity at 100 ° C (measured according to AFNOR NFT 60-100 standard): 0.56.10-2 m2 / s,
  • - "Conradson" residue (measured according to AFNOR NFT 60-116 standard): 23% by weight,
  • - content of:
  • * asphaltenes (measured according to standard AFNOR NFT 60-115): 16% by weight,
  • * sulfur (measured by fluorescence -X): 5.5% by weight,
  • * nickel (measured by X-ray fluorescence): 43 ppm,
  • * vanadium (measured by X-ray fluorescence): 138 ppm

Cette charge est traitée dans une unité mettant en oeuvre le procédé selon l'invention du type de celle présentée sur la figure 1.This charge is treated in a unit implementing the method according to the invention of the type presented in FIG. 1.

On utilise dans l'unité des solvants C3-C5 dont les compositions sont données dans le tableau 1 ci-après.

Figure imgb0009
Solvents C 3 -C 5 are used in the unit, the compositions of which are given in Table 1 below.
Figure imgb0009

Les conditions opératoires sont données dans le tableau II ci-après.

Figure imgb0010
The operating conditions are given in Table II below.
Figure imgb0010

Après séparation du solvant des différents produits, le bilan final obtenu est donné dans le tableau III ci-après.

Figure imgb0011
After separation of the solvent from the various products, the final balance obtained is given in Table III below.
Figure imgb0011

Les caractéristiques des produits obtenus sont données dans le tableau IV ci-après.

Figure imgb0012
The characteristics of the products obtained are given in Table IV below.
Figure imgb0012

Ce tableau montre bien l'intérêt du procédé selon l'invention, qui permet d'obtenir des asphaltènes très durs et une huile utilisable comme charge de craquage catalytique, car ayant un résidu, "Conradson" inférieur à 8.This table clearly shows the advantage of the process according to the invention, which makes it possible to obtain very hard asphaltenes and an oil which can be used as catalytic cracking charge, since having a residue, "Conradson" less than 8.

EXEMPLE 2EXAMPLE 2

Cet exemple concerne le traitement d'une charge hydrocarbonée constituée par le résidu de la distillation sous pression atmosphérique de l'effluent de la viscoréduction d'un résidu de la distillation sous pression réduite d'un pétrole brut SAFANIYA.This example relates to the treatment of a hydrocarbon feedstock constituted by the residue from the distillation under atmospheric pressure of the visbreaking effluent from a residue from the distillation under reduced pressure of a SAFANIYA crude oil.

Les caractéristiques de cette charge sont les suivantes :

  • - masse volumique à 15°C (mesurée selon la norme AFNOR NFT 60-101) : 1 060 kg/m3,
  • - viscosité à 100°C (mesurée selon la norme AFNOR NFT 60-100) : 0,17.10-2 m2/s,
  • - résidu "Conradson" (measurée selon la norme AFNOR NFT 60-116) : 27 % en poids,
  • - teneur en :
  • * asphaltènes (mesurée selon la norme AFNOR NFT 60-115) : 22 % en poids,
  • * soufre (mesurée par fluorescence X) : 6,2 % en poids,
  • * nickel (mesurée par fluorescence X) : 53 p.p.m.,
  • * vanadium (mesurée par fluorescence X) : 175 p.p.m.
The characteristics of this charge are as follows:
  • - density at 15 ° C (measured according to AFNOR NFT 60-101 standard): 1,060 kg / m3,
  • - viscosity at 100 ° C (measured according to AFNOR NFT 60-100 standard): 0.17.10-2 m2 / s,
  • - "Conradson" residue (measured according to AFNOR NFT 60-116 standard): 27% by weight,
  • - content of:
  • * asphaltenes (measured according to AFNOR NFT 60-115 standard): 22% by weight,
  • * sulfur (measured by X-ray fluorescence): 6.2% by weight,
  • * nickel (measured by X-ray fluorescence): 53 ppm,
  • * vanadium (measured by X-ray fluorescence): 175 ppm

Cette charge est traitée dans une unité mettant en oeuvre le procédé selon l'invention du type de celle représentée sur la figure 1.This load is treated in a unit implementing the method according to the invention of the type shown in FIG. 1.

On utilise dans l'unité des solvants C3-C5 de compositions identiques à celles des solvants de l'Exemple 1.Solvents C 3 -C 5 are used in the unit with compositions identical to those of the solvents of Example 1.

Les conditions opératoires sont données dans le tableau V ci-après.

Figure imgb0013
The operating conditions are given in Table V below.
Figure imgb0013

Après séparation du solvant des -différents produits, le bilan final obtenu est donné dans le tableau VI ci-après:

Figure imgb0014
After separation of the solvent from the different products, the final balance obtained is given in Table VI below:
Figure imgb0014

Les caractéristiques des produits obtenus sont données dans le tableau VII ci-après:

Figure imgb0015
The characteristics of the products obtained are given in Table VII below:
Figure imgb0015

Ce tableau montre bien l'intérêt du procédé selon l'invention, qui permet d'obtenir des asphaltènes très durs et une huile utilisable comme charge de craquage catalytique, car ayant un résidu "Conradson" inférieur à 8.This table clearly shows the advantage of the process according to the invention, which makes it possible to obtain very hard asphaltenes and an oil which can be used as catalytic cracking charge, since it has a "Conradson" residue of less than 8.

EXEMPLE 3EXAMPLE 3

Cet exemple concerne le traitement d'une charge hydrocarbonée constituée par le résidu de la distillation sous pression réduite du résidu de la distillation sous pression atmosphérique d'un pétrole brut d'origine Irak.This example relates to the treatment of a hydrocarbon feedstock constituted by the residue of the distillation under reduced pressure of the residue of the distillation under atmospheric pressure of a crude oil of Iraq origin.

Les caractéristiques de cette charge sont les suivantes :

  • - masse volumique à 15°C (mesurée selon la norme AFNOR NFT 60-101) : 1 016 kg/ m3,
  • - viscosité à 100°C (mesurée selon la norme AFNOR NFT 60-100) : 900 10-e m2/s
  • - résidu "Conradson" (mesurée selon la norme AFNOR NFT 60-116) : 17 % en poids,
  • - teneur en :
  • * asphaltènes (mesurée selon la norme AFNOR NFT 60-115) : 6 % en poids,
  • * soufre (mesurée par fluorescence X) : 4,9 % en poids,
  • * nickel (mesurée par fluorescence X) : 43 p.p.m.,
  • * vanadium (mesurée par fluorescence X) : 102 p.p.m.
The characteristics of this charge are as follows:
  • - density at 15 ° C (measured according to AFNOR NFT 60-101 standard): 1016 kg / m 3 ,
  • - viscosity at 100 ° C (measured according to AFNOR NFT 60-100): 900 10-e m2 / s
  • - "Conradson" residue (measured according to AFNOR NFT 60-116): 17% by weight,
  • - content of:
  • * asphaltenes (measured according to AFNOR NFT 60-115 standard): 6% by weight,
  • * sulfur (measured by X-ray fluorescence): 4.9% by weight,
  • * nickel (measured by X-ray fluorescence): 43 ppm,
  • * vanadium (measured by X-ray fluorescence): 102 ppm

Cette charge est traitée dans une unité mettant en oeuvre le procédé selon l'invention du type de celle représentée sur la figure 1.This load is treated in a unit implementing the method according to the invention of the type shown in FIG. 1.

On utilise dans l'unité des solvants C3-C6 dont les compositions sont données dans le tableau VIII ci-après.

Figure imgb0016
Les conditions opératoires sont données dans le tableau IX ci-après.
Figure imgb0017
Solvents C 3 -C 6 are used in the unit, the compositions of which are given in Table VIII below.
Figure imgb0016
The operating conditions are given in Table IX below.
Figure imgb0017

Après séparation du solvant des différents produits, le bilan final obtenu est donné dans le tableau X ci-après.

Figure imgb0018
After separation of the solvent from the various products, the final balance obtained is given in Table X below.
Figure imgb0018

Les caractéristiques des produits obtenus sont données dans le tableau XI ci-après.

Figure imgb0019
The characteristics of the products obtained are given in Table XI below.
Figure imgb0019

Ce tableau montre bien l'intérêt du procédé selon l'invention, qui permet d'obtenir des asphaltènes très durs et une huile utilisable comme charge de craquage catalytique, car ayant un résidu "Conradson" inférieur à 8.This table clearly shows the advantage of the process according to the invention, which makes it possible to obtain very hard asphaltenes and an oil which can be used as catalytic cracking charge, since it has a "Conradson" residue of less than 8.

EXEMPLE 4EXAMPLE 4

Cet exemple concerne le traitement d'une charge hydrocarbonée constituée par le résidu de la distillation sous pression réduite du résidu de la distillation sous pression atmosphérique d'un pétrole brut d'origine SAFANIYA.This example concerns the treatment of a hydrocarbon feedstock constituted by the residue from the distillation under reduced pressure of the residue from the distillation under atmospheric pressure of a crude oil of SAFANIYA origin.

Les caractéristique de cette charge sont les suivantes :

  • - masse volumique à 15°C (mesurée selon la norme AFNOR NFT 60-101) : 1 035 kg/m3,
  • - viscosité à 100°C (mesurée selon la norme AFNOR NFT 60-100) : 5 600 10-6 m2/s
  • - résidu "Conradson" (mesurée selon la norme AFNOR NFT 60-116) : 23 % en poids,
  • - teneur en :
  • * asphaltènes (mesurée selon la norme AFNOR NFT 60-115) : 16 % en poids,
  • * soufre (mesurée par fluorescence X) : 5,5 % en poids,
  • *nickel (mesurée par fluorescence X) : 43 p.p.m.,
  • *vanadium (mesurée par fluorescence X) : 138 p.p.m.
The characteristics of this load are as follows:
  • - density at 15 ° C (measured according to AFNOR NFT 60-101 standard): 1035 kg / m 3 ,
  • - viscosity at 100 ° C (measured according to AFNOR NFT 60-100 standard): 5,600 10 -6 m 2 / s
  • - "Conradson" residue (measured according to AFNOR NFT 60-116 standard): 23% by weight,
  • - content of:
  • * asphaltenes (measured according to AFNOR NFT 60-115 standard): 16% by weight,
  • * sulfur (measured by X-ray fluorescence): 5.5% by weight,
  • * nickel (measured by X-ray fluorescence): 43 ppm,
  • * vanadium (measured by X-ray fluorescence): 138 ppm

Cette charge est traitée dans une unité mettant en oeuvre le procédé selon l'invention du type de celle présentée sur la figure 2.This charge is treated in a unit implementing the method according to the invention of the type presented in FIG. 2.

On utilise dans l'unité des solvants C3-C5 dont les compositions sont données dans le tableau XII ci-après.

Figure imgb0020
Les conditions opératoires sont données dans le tableau XIII ci-après.
Figure imgb0021
Solvents C 3 -C 5 are used in the unit, the compositions of which are given in Table XII below.
Figure imgb0020
The operating conditions are given in Table XIII below.
Figure imgb0021

Après séparation du solvant des différents produits, le bilan final obtenu est donné dans le tableau XIV ci-après.

Figure imgb0022
After separation of the solvent from the various products, the final balance obtained is given in Table XIV below.
Figure imgb0022

Les caractéristiques des produits obtenus sont données dans le tableau XV ci-après.

Figure imgb0023
The characteristics of the products obtained are given in Table XV below.
Figure imgb0023

Ce tableau montre bien l'intérêt du procédé selon l'invention, qui permet d'obtenir des asphaltènes très durs et une huile utilisable comme charge de craquage catalytique, car ayant un résidu "Conradson" inférieur à 8.This table clearly shows the advantage of the process according to the invention, which makes it possible to obtain very hard asphaltenes and an oil which can be used as catalytic cracking charge, since it has a "Conradson" residue of less than 8.

Claims (10)

1. Process for the elimination of asphaltenes from a heavy hydrocarbon feedstock, said process leading to the obtaining:
- of a de-asphalted oily phase with a "Conradson" index equal to or less than 10,
- of a "resins" fraction,
- of an "asphaltenes" fraction whose softening point is equal to or higher than 150°C, said process comprising two stages of precipitation from the feedstock, firstly of the "asphaltenes" fraction alone, and secondly of the "resins" fraction, in certain cases accompanied by the "asphaltenes" fraction, by means, respectively, of a heavy solvent and a light solvent, said process being characterised in that the heavy solvent contains from 5 to 40% by volume of a hydrocarbon with 3 carbon atoms and 60 to 95% of at least one hydrocarbon with 5 carbon atoms and the light solvent contains from 20 to 80% by volume of a hydrocarbon with 3 carbon atoms and from 20 to 80% by volume of at least one hydrocarbon with at least 5 carbon atoms, the proportion of the hydrocarbon containing 3 carbon atoms being higher in the light solvent than in the heavy solvent.
2. Process according to claim 1, characterized in that it comprises two stages:
a) a first stage of precipitation from the feedstock, by means of a heavy solvent, of the "asphaltenes" fraction, said first stage leading to the obtaining:
- on the one hand, of the "asphaltenes" fraction, after separation of the solvent which it contains,
- on the other, of a solution in the heavy solvent of the "resins" fraction and the oily phase;
b) a second stage of precipitation from the solution obtained in stage a), by means of a light solvent, of the "resins" fraction, said second stage leading to the obtaining:
- on the one hand, of the "resins" fraction, after separation of the solvent which it contains,
- on the other, of the de-asphalted oily phase, after separation of the light solvent in which it is in solution.
3. Process according to claim 2, characterized in that the light solvent used for the precipitation of the "resins" fraction is obtained by combining the heavy solvent contained in the solution obtained at the conclusion of stage a) with a third solvent lighter than the light solvent, said third solvent being obtained during the separation of the light solvent from the oily phase by preferential vaporization of the hydrocarbon with 3 carbon atoms, said vaporization leading to the obtaining of said third solvent and a heavy solvent recycled to the first stage of precipitation of the "asphaltenes" fraction.
4. Process according to claim 3, characterized in that the content in the hydrocarbon with 3 carbon atoms of the third light solvent is augmented by refluxes used during the separation of the de-asphalted oil and the light solvent.
5. Process according to any one of claims 2 to 4, characterized in that:
a) the heavy solvent used in the first stage contains from 10 to 40% by volume of hydrocarbon with 3 carbon atoms and from 60 to 90% by volume of at least one hydrocarbon with at least 5 carbon atoms and, preferably, from 15 to 35% by volume of hydrocarbon with 3 carbon atoms and from 65 to 85% by volume of at least one hydrocarbon with at least 5 carbon atoms,
b) the light solvent used in the second stage contains from 20 to 80% by volume of hydrocarbon with 3 carbon atoms and from 20 to 80% by volume of at least one hydrocarbon with at least 5 carbon atoms and, preferably, from 25 to 75% by volume of hydrocarbon with 3 carbon atoms and from 25 to 75% by volume of at least one hydrocarbon with at least 5 carbon atoms.
6. Process according to claim 1, characterized in that it comprises two stages:
a') a first stage of precipitation from the feedstock, by means of a iight solvent, of the "resins" and "asphaltenes" fractions, said first stage leading to the obtaining:
- on the one hand, of a mixture of the "resins" and "asphaltenes" fractions containing some light solvent,
- on the other, of the de-asphalted oily phase, after separation of the light solvent in which it is in solution and which is reused in the first stage;
b') a second stage of treatment of the mixture of the "resins" and "asphaltenes" fractions by means of the heavy solvent, leading to the obtaining after dissolution of the "resins" fraction in the heavy solvent:
- on the one hand, of the "resins" fraction, after separation of the heavy solvent in which it is in solution;
- on the other, of the "asphaltenes" fraction, after separation of the solvent which it contains.
7. Process according to claim 6, characterized in that the light solvent used for the precipitation of the "resins" and "asphaltenes" fractions is obtained by combining the light solvent recycled at the conclusion of stage a') with the light solvent obtained during the separation of the heavy solvent from the "resins" fraction by preferential vaporization of the hydrocarbon with 3 carbon atoms, said vaporization leading to the obtaining of said light solvent and a solvent heavier than the heavy solvent, which is used to reconstitute the heavy solvent used in the second stage in combination with the light solvent contained in the mixture of the "resins" and "asphaltenes" fractions obtained at the conclusion of stage a').
8. Process according to any one of claims 6 and 7, characterized in that:
a) the light solvent used in the first stage contains from 20 to 80% by volume of hydrocarbon with 3 carbon atoms and from 20 to 80% by volume of at least one hydrocarbon with at least 5 carbon atoms and, preferably, from 30 to 70% by volume of at least one hydrocarbon with 3 carbon atoms and from 30 to 70% of at least one hydrocarbon with at least 5 carbon atoms,
b) the heavy solvent used in the second stage contains from 5 to 30% by volume of hydrocarbon with 3 carbon atoms and from 70 to 95% by volume of at least one hyrocarbon with at least 5 carbon atoms and, preferably, from 10 to 25% by volume of hydrocarbon with 3 carbon atoms and from 75 to 90% of at least one hydrocarbon with at least 5 carbon atoms.
9. Process according to any one of claims 1 to 8, characterized in that the hydrocarbons with 3 carbon atoms and with at least 5 carbon atoms are respectively propane and pentane.
10. Process according to any one of claims 1 to 8, characterized in that the hydrocarbons with 3 carbon atoms and with at least 5 carbon atoms are respectively propane and hexane.
EP87401091A 1986-05-15 1987-05-14 Process for the elimination of asphaltenes from a hydrocarbon feedstock Expired - Lifetime EP0246956B1 (en)

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Application Number Priority Date Filing Date Title
FR8606994A FR2598716B1 (en) 1986-05-15 1986-05-15 PROCESS FOR DEASPHALTING A HEAVY HYDROCARBON LOAD
FR8606994 1986-05-15

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EP0246956A1 EP0246956A1 (en) 1987-11-25
EP0246956B1 true EP0246956B1 (en) 1990-11-28

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EP (1) EP0246956B1 (en)
JP (1) JP2525409B2 (en)
CA (1) CA1330063C (en)
DE (1) DE3766415D1 (en)
FR (1) FR2598716B1 (en)

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DE3766415D1 (en) 1991-01-10
US4810367A (en) 1989-03-07
FR2598716A1 (en) 1987-11-20
FR2598716B1 (en) 1988-10-21
JP2525409B2 (en) 1996-08-21
CA1330063C (en) 1994-06-07
JPS62273289A (en) 1987-11-27
EP0246956A1 (en) 1987-11-25

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