EP0201364B1 - Procédé de désasphaltage d'une charge d'hydrocarbures contenant des asphaltènes - Google Patents

Procédé de désasphaltage d'une charge d'hydrocarbures contenant des asphaltènes Download PDF

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Publication number
EP0201364B1
EP0201364B1 EP86400589A EP86400589A EP0201364B1 EP 0201364 B1 EP0201364 B1 EP 0201364B1 EP 86400589 A EP86400589 A EP 86400589A EP 86400589 A EP86400589 A EP 86400589A EP 0201364 B1 EP0201364 B1 EP 0201364B1
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EP
European Patent Office
Prior art keywords
solvent
phase
charge
mixture
process according
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Expired
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EP86400589A
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German (de)
English (en)
French (fr)
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EP0201364A1 (fr
Inventor
Jean-François Le Page
Alain Billon
Frédéric Morel
Pierre Renard
Jean-Michel Biedermann
Michel Laborde
Jacques Bousquet
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IFP Energies Nouvelles IFPEN
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IFP Energies Nouvelles IFPEN
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
    • C10G21/003—Solvent de-asphalting
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents

Definitions

  • the process which is the subject of the present invention applies to the treatment of residues of conventional crude oils, whether atmospheric residues or residues under vacuum, as well as to the treatment of heavy or extra heavy oils topped such as they can be obtained, for example, from the deposits of FAJA PETROLIFERA in VENEZUELA or from the deposits of ATHABASCA in CANADA.
  • the method as claimed can also be advantageously used for the treatment of atmospheric or vacuum residues which result from another thermal or catalytic preliminary treatment such as visbreaking, hydroviscoreduction, heat treatment in the presence of a hydrogen donor solvent, various catalytic hydrotreatments with more or less extensive conversion of the charge treated.
  • This separation consists in breaking the balance existing between the asphaltenes and the surrounding maltenic medium by adding a solvent which decreases the viscosity and especially the surface tension of the oily medium.
  • the recommended solvents are generally paraffins or (and) light olefins with 3, 4, 5, 6, and (or) 7 carbon atoms. In fact, light paraffin plays an anti-solvent role with respect to asphaltenes and possibly with respect to resins.
  • Asphaltenes and resins are rejected out of the oily medium in the form of a distinct phase and this all the better when the density and the surface tension of the solvent medium plus oil are lower. Consequently, the yield in "asphalt phase" and the quality of the deasphalted oil are linked for a given charge to the following parameters and variables: nature of the solvent, solvent content, temperature and pressure, but also very strongly depend on the characteristics of the technology. used.
  • the process which the subject of the present invention therefore relates to deasphalting with hydrocarbon solvents comprising paraffinic or olefinic hydrocarbons having from 3 to 7 carbon atoms.
  • hydrocarbon solvents comprising paraffinic or olefinic hydrocarbons having from 3 to 7 carbon atoms.
  • the use of the hydrocarbon solvent is carried out in such a way that it makes it possible to obtain excellent yields of a very good quality oil with a minimum solvent content and that it makes it possible to design industrial extrapolation to units capable of processing annual capacities of around 2 to 4 million tonnes in a single line.
  • a first object of the present invention is to carry out the deasphalting of a hydrocarbon charge containing asphaltenes in particular of a residue or of a heavy oil, with a solvent having from 3 to 7 carbon atoms, used in a ratio solvent / charge volume from 2.5 / 1 to 6/1, so as to obtain an oil containing less than 0.05% of asphaltenes precipitated by heptane according to AFNOR NFT 60115 standard.
  • a second object of the invention is to selectively carry out the operation, that is to say to obtain, concurrently with the quality of the deasphalted oil, a very good yield in this same oil and this by implementing the minimum solvent, i.e. metric solvent / oil volumetric ratios which may be as low as 3/1 to 4/1.
  • a third object of the invention consists in carrying out the operation by separating the elementary physicochemical operations which make up the overall deasphalting operation: mixing-precipitation, decantation of the asphalt phase, washing-peptization of the asphalt phase.
  • the process which is the subject of the invention allows the treatment of very large annual residues or heavy oils in a single decanter with respect for the quality and yield criteria which constitute the first and second subject of the invention.
  • US-A 2,002,004, 2,101,308 and 3,074,882 they recommend carrying out the deasphalting operation in two or more successive stages but the sequences of stages envisaged are conceptually different from the staggering of stages of the present invention.
  • US Pat. No. 2,002,004 relates to a two-stage deasphalting process with intermediate distillation of the hydrocarbon phase rich in solvent originating from the first extraction zone. The effluent from the bottom of the distillation column is subjected to a second deasphalting step which in fact makes it possible to isolate resins.
  • the patent US-A 2 101 308 proposes a first step of deasphalting with light gasoline as solvent; the light oil-essence mixture from this first is treated with SO 2 , for a subsequent elimination of resins and aromatics.
  • US-A 3,074,882 operates a first butane precipitation.
  • the butane is separated from the oil-butane mixture and the residual oil is treated with propane in two successive stages making it possible, on the one hand, to obtain resins and, on the other hand, a deasphalted and de-resinated oil.
  • the asphaltic phase washing solvent is the same as that used for the precipitation.
  • the mixture between the charge to be deasphalted and the deasphalting solvent is produced upstream of the exchanger which raises the mixing temperature to the value required to achieve good precipitation and good decantation.
  • the charge-solvent mixture passes through the tubes of the exchanger and not on the shell side.
  • the residence time of the charge-solvent mixture in the precipitation mixing zone is between 5 sec and 5 min, preferably between 20 seconds and 120 seconds.
  • the residence time of the mixture in the settling zone is between 4 and 20 minutes.
  • the residence time of the oil-solvent mixture in the washing zone also remains between 4 and 20 minutes.
  • the upward speeds of the oil-solvent mixtures both in the settling zone and in the washing zone will usefully remain less than 1 cm / s and preferably less than 0.5 cm / s.
  • the temperature applied in the washing zone will be 5 to 50 ° C lower than the temperature applied in the decanting zone.
  • the oil-solvent mixture from the washing zone will be recycled in the decanter and even more advantageously upstream from the exchanger located at the entrance to the decantation zone.
  • the solvent / asphalt phase ratio recommended in the washing zone will be between 0.5 and 8 and preferably between 1 and 5.
  • the process can comprise two stages, each stage including the three basic stages of precipitation, decantation and washing.
  • the temperature recommended in each stage of the first stage is preferably on average 10 to 40 ° C lower than the temperature of each corresponding stage of the second stage.
  • the process which is the subject of the invention can use hydrocarbon solvents having from 3 to 7 carbon atoms, paraffinic, olefinic or cyclanic, alone, mixed together in various proportions or added with additives, for example, of the type phenol, glycol, alcohols from C1 to C6.
  • the process of the present invention lends itself more advantageously to the use of paraffinic and / or olefinic solvents having from 4 to 6 carbon atoms.
  • FIG. 1 presents the essential characteristics of the method corresponding to the invention.
  • the load to be treated is introduced via line (1) to the mixing valve (2), where the solvent S1 and S "1 is introduced, originating from the recovery of the solvent (23) contained respectively in the solvent mixture. - oil or in the solvent-asphalt phase mixture (lines 3 and 4).
  • the charge-solvent mixture passes through an exchanger (5) where it is brought to the temperature required for the deasphalting operation considered; this temperature will vary between 100 and 220 ° C according to the solvent considered (for example isobutane, butane, isopentane, pentane, light gasoline) according to the type of feed to be treated (headless crude, atmospheric residue, vacuum residue), according to the origin of the crude oil considered and according to the solvent / oil ratio used.
  • the solvent considered for example isobutane, butane, isopentane, pentane, light gasoline
  • the temperature at outlet of the exchanger will be between 190 and 170 ° C and the pressure between 4 and 5 M Pascals da ns to the extent that one aims to obtain a deasphalted oil containing less than 0.05% of asphalts according to the AFNOR NFT 60115 STANDARD. It is important to specify that according to one of the preferred characteristics of the process, the charge-solvent mixture passes in the exchanger tubes and not on the shell side, in addition, it is recommended to carry out a gravity flow in this exchanger, that is to say that the charge-solvent mixture travels up and down the exchanger tubes .
  • the mixture brought to the required temperature is introduced via line (6) into the extractor flask (7) where the decantation takes place.
  • the precipitation of the asphalt phase begins almost instantaneously at the level of the mixing valve and is followed in the exchanger (5) as the temperature rises.
  • the residence time of the mixture between the mixing valve and the entry of the settling tank is between 5 seconds and 5 minutes and preferably between 20 seconds and 120 seconds.
  • the turbulence in line 6 is usefully controlled to avoid the bursting into too small particles of the micelles of asphaltic phase in suspension in the oil-solvent medium; in practice, it is recommended that at the outlet of the exchanger the number of REYNOLDS in the mixture be between 2.104 and 106 and preferably between 5.104 and 5.105. In this range of values, it can also be seen that the agglomeration of the micelles is initiated, making subsequent settling in the settling tank easier and faster.
  • the asphaltic phase micelles are agglomerated and decanted.
  • the volume and the geometry of the decanter are calculated so that the residence time of the solvent-oil mixture is between 4 and 20 minutes and preferably between 8 and 15 minutes and so that the rate of rise of the solvent-oil mixture is always less than 1 cm per second.
  • the ball decanter preferably operates in an isothermal manner, that is to say at a temperature substantially equal to the inlet temperature of the mixture, apart from the heat losses.
  • the asphalt phase is collected in an underlying boot (8) where a level control causes it to be drawn off by the pump (10) via the pipes (9 and 11) up to the column (12) where the washing of the asphaltic phase and the selective repeptisation of part of the resins by the solvent S'1 recycled from the fractionation unit (23) via the pipe (14).
  • the exchanger (15) makes it possible to adjust the temperature of the washing solvent to the optimum temperature for the envisaged operation.
  • the pressure applied in the washing tower is preferably very close to the upstream decanter pressure; the temperature of the solvent S'1 at the entrance to the tower will preferably be 5 to 50 ° C lower than the temperature of the asphalt phase introduced by line (11) at the top of the washing zone.
  • the temperature gradient established between the inlets of the pipes (11) and (14) makes it possible to adjust for a given solvent flow rate S'1 and an asphaltic phase of a given nature the rate of repeptation of the resins, that is to say -dith allows to regulate the asphalt yield and the softening point of the asphalt.
  • the solvent flow rate also affects the asphalt yield and its softening point. According to the process which is the subject of the invention, this flow rate is adjusted so that the volume ratio of solvent / asphalt phase is between 0.5 and 8 and preferably between 1 and 5.
  • the column is advantageously operated so that the level of settling of the asphalt phase (17) is adjusted below the injection pipe (14) of the solvent S'1 and more precisely below the distribution device ( 16) of this same solvent in the continuous solvent-oil medium although a setting at a higher level still gives good performance.
  • the column is preferably equipped with baffle plates (13) which allow better contact between the micelles of the asphalt phase and the upward flow of solvent. These baffles are preferably calculated in such a way that the rate of rise of the solvent or more precisely of the solvent phase added with the washed oil and the peptized resins remains less than 36 m / hour.
  • the column head is preferably devoid of baffles to reduce this rate of rise and can be designed with a slightly larger diameter to avoid any entrainment of the colloidal particles of asphalt phase of diameter less than one micron.
  • the product from the top of the column is recycled in the liquid phase via the line (18) in the solvent S1 slightly upstream of the mixing valve (2).
  • the asphalt phase swollen with almost pure solvent is withdrawn from the bottom of the washing column by means of the pump (20) via the line (19) up to the vaporization tower (21) where the asphalt, which has been withdrawn, is separated. via the line (22), solvent which is recycled via the line (4), either at the top of the decanter, or upstream of this decanter and preferably at the level of the mixing valve.
  • solvent which is recycled via the line (4) either at the top of the decanter, or upstream of this decanter and preferably at the level of the mixing valve.
  • the recovery of the solvent associated with the deasphalted oil it is shown diagrammatically by the rectangle (23) and can for example be carried out in the process relating to the invention by vaporization of the solvent in a cascade of evaporators or of the exchanger type. conventional, either preferably of the falling film exchanger type or by separation of the solvent phase from the oil phase in a decanter operating under supercritical conditions or by ultrafiltration of the solvent on appropriate mineral membranes.
  • the decanter was in elongated form, was provided with a boot and was preferably inclined by 5 to 10 ° relative to the horizontal plane to allow the asphalt phase to flow freely towards the boot underlying.
  • the invention does not however stipulate that this decanter is necessarily elongated; it can also be vertical as shown in FIG. 2, insofar as this geometry makes it possible to comply with the constraints of rising speed and of settling time recommended above. This geometry which requires less floor space will therefore be recommended for the treatment of annual capacities of less than 2 million tonnes:
  • the decanter is, for process conditions, arranged vertically, the arrangement of the stages and the operating conditions recommended are strictly those which are the subject of the present invention.
  • the method in a last variant can also be applied to the case where the operation is carried out in two stages with precipitation of a hard asphalt phase in a first stage and precipitation of a resin phase in a second stage.
  • the simple idea of separate production of an asphalt phase and a resin phase has been known and practiced industrially for a very long time and is not part of the body of the invention.
  • the object of the invention relates to the fact that each stage, as shown in FIG. 3, comprises a staggering of the 3 elementary stages: mixing-precipitation, decantation, washing-repeping, completely similar to that described in the previous variants where the asphalts and resins were precipitated in a single phase.
  • the precipitation and decantation are carried out in the first stage at a temperature of 20 to 60 ° C lower than that which is applied when the precipitation is carried out in one go, that is to say say at the minimum temperature so that the asphalt phase remains liquid and sufficiently fluid at the outlet of the decanter to be able to be handled without problem.
  • the step of washing the asphalt phase in this variant is carried out at a temperature equal to or slightly higher than that of the decanter.
  • the solvent-oil-resin mixture from washing through line 18 is mixed with the solvent-oil-resin mixture from the first decanter (24).
  • the oil-resin solvent mixture is heated (35) to a temperature 30 to 70 ° C higher than that applied in the first decanter.
  • the solvent-oil-resins mixture preferably passes through the tubes of the exchanger and not on the shell side; moreover the flow of the solvent-oil-resins mixture will be a gravity flow; the extract is separated by the line (38) for fractionation in the separator (23).
  • the raffinate is sent by line (39) to the washer (40).
  • the ascending speeds and the residence times in the settling tank (37) and the column (40) are included in the ranges recommended above for the tank (7) and the column (12).
  • the solvent / resin phase ratio at (40) is between 2 and 4.
  • the solvent-oil mixture is recycled via line (43) upstream of the exchanger (35).
  • the solvent for washing the resin phase is injected through line (41) at the bottom of the column (40) for washing the resin phase after passing through the exchanger (42) so as to adjust the temperature of said solvent to a value lower than that of the decanter (37) by 5 to 30 ° C.
  • the resin phase (44) is released from the solvent entrained in (45) by "flash” and / or steam entrainment.
  • the resin phase (46) is recovered.
  • the recovered solvent is sent via line (47) to the pipe (4).
  • the process therefore makes it possible, in two stages of similar designs, to very flexibly ensure the production of an oil phase (27) devoid of asphaltenes and very poor in resins as well as the simultaneous production of an asphaltic phase and a resin phase, the proportions of these last two phases can be adjusted at will, for a given charge, a solvent and given solvent levels, by the choice of the temperatures applied in (7) and (37) on the one hand, in (15) and (42) on the other hand.
  • a SAFANIYA residue is deasphalted by addition of a solvent essentially consisting of a mixture of pentane and isopentane.
  • the characteristics of the residue are presented in Table 1 and the composition of section C5 in Table 2.
  • the operation is carried out in a unit capable of treating from 1 t / h to 3 t / h of residue and whose process characteristics are similar to those which are the subject of the invention described above.
  • the tubular exchanger is arranged vertically.
  • the washing-repeptation column is equipped with crossed horizontal baffles so as to achieve the equivalent of 2 theoretical stages for both mass and heat transfer.
  • a series of 10 tests were carried out in accordance with the diagram in FIG. 1.
  • the operating conditions applied are presented in Table 3.
  • Table 3 In this series of tests the solvent of the oil-solvent mixture was recovered for 90% in a cascade of falling film evaporators and for the last 10 percent by stripping of the oily phase under pressure conditions lower than those applied in the decanting operation.
  • Table 4 gives the yields and some characteristics of the products obtained.
  • the deasphalting of a BOSCAN atmospheric residue is carried out by adding the same solvent of the C5 cut type as that used in Example 1.
  • the operation is carried out in the same unit as that described in connection with Example 1.
  • Table 6 gives the essential characteristics of the charge treated and Table 7 the yields and characteristics of the products obtained.
  • This example was more particularly chosen to illustrate the importance of the washing step on the yields of desasperated oil. This series of tests further highlights the importance of the conditions applied in the washing step.
  • the oil yields are higher the lower the washing temperature and the higher the solvent / asphalt phase ratio.
  • the volume of asphalt phase which, at the outlet of the decanter, is composed of the asphalt swollen with solvent and oil, is between 1.6 and 2 times the volume of the final asphalt which leaves the washing tower. This implies that the ratio of the solvent to the asphalt phase entering the washing tower in the previous tests remains well between 0.5 and 8.
  • the deasphalting of the SAFANIYA vacuum residue is carried out, the characteristics of which are presented in Table 1 but using for the precipitation a C4 cut containing by weight 3% of propane, 35% of isobutane, 61% of butane and 1% of isopentane.
  • the tests are carried out in the same unit as that described in the previous examples.
  • the operating conditions of the series of tests are summarized in Table 8, the yields and characteristics of the products obtained are presented in Table 9.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Working-Up Tar And Pitch (AREA)
EP86400589A 1985-04-05 1986-03-19 Procédé de désasphaltage d'une charge d'hydrocarbures contenant des asphaltènes Expired EP0201364B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8505350A FR2579985B1 (zh) 1985-04-05 1985-04-05
FR8505350 1985-04-05

Publications (2)

Publication Number Publication Date
EP0201364A1 EP0201364A1 (fr) 1986-11-12
EP0201364B1 true EP0201364B1 (fr) 1989-01-18

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EP86400589A Expired EP0201364B1 (fr) 1985-04-05 1986-03-19 Procédé de désasphaltage d'une charge d'hydrocarbures contenant des asphaltènes

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US (1) US4715946A (zh)
EP (1) EP0201364B1 (zh)
JP (1) JPH0613714B2 (zh)
KR (1) KR930005527B1 (zh)
CN (1) CN1016965B (zh)
CA (1) CA1280990C (zh)
DE (1) DE3661840D1 (zh)
ES (1) ES8703508A1 (zh)
FR (1) FR2579985B1 (zh)
MX (1) MX168799B (zh)

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US7594990B2 (en) 2005-11-14 2009-09-29 The Boc Group, Inc. Hydrogen donor solvent production and use in resid hydrocracking processes
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US10590360B2 (en) 2015-12-28 2020-03-17 Exxonmobil Research And Engineering Company Bright stock production from deasphalted oil
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IT201700035782A1 (it) * 2017-03-31 2018-10-01 Eni Spa Metodo per la separazione fisica di correnti di spurgo da raffineria.
FR3075809B1 (fr) 2017-12-21 2020-09-11 Ifp Energies Now Procede de conversion de charges lourdes d’hydrocarbures avec recycle d’une huile desasphaltee
US11084985B2 (en) * 2018-06-01 2021-08-10 Exxonmobil Research And Engineering Company Boiling free fractionation of hydrocarbon streams utilizing a membrane cascade
KR20210039743A (ko) * 2019-10-02 2021-04-12 현대오일뱅크 주식회사 초저황 연료유의 제조방법 및 그로부터 얻어지는 초저황 연료유
FR3113062B1 (fr) 2020-07-30 2023-11-03 Ifp Energies Now Procédé d’hydroconversion de résidus à plusieurs étages d’hydroconversion intégrant une étape de désasphaltage
FR3113678B1 (fr) 2020-08-31 2022-08-12 Ifp Energies Now Bitumes comportant des bases bitumes non conventionnelles
FR3130836A1 (fr) 2021-12-20 2023-06-23 IFP Energies Nouvelles Hydroconversion en lit bouillonnant ou hybride bouillonnant-entraîné d’une charge comportant une fraction plastique
FR3133197A1 (fr) 2022-03-01 2023-09-08 IFP Energies Nouvelles Hydroconversion en lit bouillonnant ou hybride bouillonnant-entraîné d’une charge comportant une fraction d’huile végétale ou animale
FR3133618A1 (fr) 2022-03-17 2023-09-22 IFP Energies Nouvelles Hydroconversion en lit bouillonnant ou hybride bouillonnant-entraîné d’une charge comportant une fraction d’huile de pyrolyse de plastiques et/ou de combustibles solides de recuperation

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Publication number Publication date
CN1016965B (zh) 1992-06-10
DE3661840D1 (en) 1989-02-23
FR2579985B1 (zh) 1988-07-15
EP0201364A1 (fr) 1986-11-12
MX168799B (es) 1993-06-08
US4715946A (en) 1987-12-29
KR930005527B1 (ko) 1993-06-22
ES553737A0 (es) 1987-02-16
CA1280990C (fr) 1991-03-05
JPH0613714B2 (ja) 1994-02-23
FR2579985A1 (zh) 1986-10-10
CN86102355A (zh) 1986-10-01
JPS61246285A (ja) 1986-11-01
ES8703508A1 (es) 1987-02-16
KR860008254A (ko) 1986-11-14

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