EP3018188B1 - Verfahren zur umwandlung von erdöleinsätzen, das eine hydrotreating-phase im festbett, eine hydrocracking-phase in einer wirbelschicht, eine reifephase und eine abscheidungsphase von sedimenten für die herstellung von heizöl mit geringem sedimentanteil umfasst - Google Patents

Verfahren zur umwandlung von erdöleinsätzen, das eine hydrotreating-phase im festbett, eine hydrocracking-phase in einer wirbelschicht, eine reifephase und eine abscheidungsphase von sedimenten für die herstellung von heizöl mit geringem sedimentanteil umfasst Download PDF

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EP3018188B1
EP3018188B1 EP15306717.8A EP15306717A EP3018188B1 EP 3018188 B1 EP3018188 B1 EP 3018188B1 EP 15306717 A EP15306717 A EP 15306717A EP 3018188 B1 EP3018188 B1 EP 3018188B1
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stage
fraction
separation
hydrocracking
hydrotreatment
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French (fr)
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EP3018188A1 (de
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Wilfried Weiss
Thibault Corre
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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
    • C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
    • 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
    • C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
    • C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
    • 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
    • C10G31/06—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for by heating, cooling, or pressure treatment
    • 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
    • C10G49/00—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00
    • C10G49/002—Apparatus for fixed bed hydrotreatment processes
    • 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
    • C10G65/00—Treatment of hydrocarbon oils by two or more hydrotreatment processes only
    • C10G65/02—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only
    • C10G65/12—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including cracking steps and other hydrotreatment steps
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1037—Hydrocarbon fractions
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1037—Hydrocarbon fractions
    • C10G2300/1048—Middle distillates
    • C10G2300/1059—Gasoil having a boiling range of about 330 - 427 °C
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/107—Atmospheric residues having a boiling point of at least about 538 °C
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1077—Vacuum residues
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • C10G2300/202—Heteroatoms content, i.e. S, N, O, P
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • C10G2300/205—Metal content
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • C10G2300/205—Metal content
    • C10G2300/206—Asphaltenes
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • C10G2300/208—Sediments, e.g. bottom sediment and water or BSW
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/30—Physical properties of feedstocks or products
    • C10G2300/301—Boiling range
    • 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
    • C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
    • C10G2400/04—Diesel oil
    • 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
    • C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
    • C10G2400/06—Gasoil

Definitions

  • the present invention relates to the refining and the conversion of heavy hydrocarbon fractions containing, inter alia, sulfur-containing impurities. It relates more particularly to a process for converting heavy petroleum feeds of the atmospheric residue type and / or vacuum residue for the production of heavy fractions that can be used as fuel bases, in particular bunker oil bases, with a low sediment content.
  • the process according to the invention also makes it possible to produce atmospheric distillates (naphtha, kerosene and diesel), vacuum distillates and light gases (C1 to C4).
  • the sediment content according to ISO 10307-1 (also known as IP375) is different from the sediment content after aging according to ISO 10307-2 (also known as IP390).
  • the sediment content after aging according to ISO 10307-2 is a much more stringent specification and corresponds to the specification for bunker fuels.
  • a ship may therefore use a sulfur-containing fuel oil if the ship is equipped with a flue gas treatment system that reduces emissions of sulfur oxides.
  • FR 2764300 and EP 0665282 describe a hydrotreatment process of heavy oils with the aim of extending the life of the reactors.
  • the process described in FR 2764300 describes a process for obtaining fuels (gasoline and diesel) having in particular a low sulfur content.
  • the fillers treated in this process do not contain asphaltenes.
  • WO 2014/096704 A1 discloses a process for treating a hydrocarbon feedstock containing at least one hydrocarbon fraction having a sulfur content of at least 0.1% by weight, an initial boiling temperature of at least 340 ° C and an end temperature boiling point of at least 440 ° C to obtain a liquid hydrocarbon fraction having a sediment content after aging less than or equal to 0.1% by weight, said process comprising the following steps: a) a hydrotreatment step in a fixed bed, in which the hydrocarbon feedstock and hydrogen are contacted on a hydrotreatment catalyst, b) an optional step of separating the effluent from step a) of hydrotreatment into at least one light hydrocarbon fraction containing fuel bases and a heavy fraction containing compounds boiling at least 350 ° C, c) a step of hydrocracking at least a portion of the effluent from step a) or from at least one party e of the heavy fraction resulting from step b), in at least one reactor containing a catalyst supported in a bubbling bed, d)
  • Fuel oils used in maritime transport generally include atmospheric distillates, vacuum distillates, atmospheric residues and vacuum residues from direct distillation or from refining processes, including hydrotreatment and conversion processes, which may be be used alone or mixed. These processes, although known to be suitable for heavy loads loaded with impurities, however, produce hydrocarbon fractions comprising catalyst fines and sediments which must be removed to satisfy a product quality such as bunker fuel oil.
  • the sediments may be precipitated asphaltenes. Initially in the feed, the conversion conditions and in particular the temperature cause them to undergo reactions (dealkylation, polymerization, etc.) leading to their precipitation. Regardless of the nature of the charge, these phenomena generally occur during the implementation of severe conditions giving rise to conversion rates (for compounds boiling above 540 ° C: 540 + ° C), ie ie greater than 30, 40 or 50%.
  • the applicant in its research has developed a new process integrating a step of maturation and sediment separation downstream of a fixed bed hydrotreating step and a hydrocracking step. Surprisingly, it has been found that such a method makes it possible to obtain liquid hydrocarbon fractions having a low sediment content after aging, said fractions being advantageously wholly or partly used as fuel oil or as fuel oil base for the future. specifications, namely and a sediment content after aging less than or equal to 0.1% by weight
  • One of the objectives of the present invention is to propose a process for converting heavy petroleum feedstocks for the production of fuel oils and fuel bases. in particular bunker oil and bunker oil bases with a low sediment content after aging less than or equal to 0.1% by weight.
  • Another object of the present invention is to jointly produce, by the same method, atmospheric distillates (naphtha, kerosene, diesel), vacuum distillates and / or light gases (C1 to C4).
  • the bases of the naphtha and diesel type can be upgraded to refineries for the production of automotive and aviation fuels, such as, for example, super-fuels, Jet fuels and gas oils.
  • the feedstock treated in the process according to the invention is preferably a hydrocarbon feed having an initial boiling point of at least 340 ° C and a final boiling point of at least 440 ° C.
  • its initial boiling point is at least 350 ° C., preferably at least 375 ° C.
  • its final boiling point is at least 450 ° C., preferably at least 450 ° C. at least 460 ° C, more preferably at least 540 ° C, and even more preferably at least 600 ° C.
  • the hydrocarbon feedstock according to the invention may be chosen from atmospheric residues, vacuum residues resulting from direct distillation, crude oils, crude head oils, deasphalting resins, asphalts or deasphalting pitches, process residues. conversion products, aromatic extracts from lubricant base production lines, oil sands or derivatives thereof, oil shales or their derivatives, source rock oils or their derivatives, whether alone or in combination.
  • the fillers being treated are preferably atmospheric residues or vacuum residues, or mixtures of these residues.
  • the hydrocarbon feedstock treated in the process may contain, among other things, sulfur-containing impurities.
  • the sulfur content may be at least 0.1% by weight, at least 0.5% by weight, preferably at least 1% by weight, more preferably at least 4% by weight, still more preferably at least 5% by weight.
  • the feedstock may contain at least 1% C7 asphaltenes and at least 5 ppm metals, preferably at least 2% C7 asphaltenes and at least 25 ppm metals.
  • This co-charge may be a hydrocarbon fraction or a lighter hydrocarbon fraction mixture, which may preferably be chosen from the products resulting from a fluid catalytic cracking (FCC) process according to the English terminology. Saxon), a light cutting oil (LCO or "light cycle oil” according to the English terminology), a heavy cutting oil (HCO or "heavy cycle oil” according to the English terminology), a decanted oil, a FCC residue, a gas oil fraction, especially a fraction obtained by atmospheric distillation or under vacuum, such as vacuum gas oil, or may come from another refining process.
  • FCC fluid catalytic cracking
  • the co-charge may also advantageously be one or more cuts resulting from the liquefaction process of the coal or the biomass, aromatic extracts, or any other hydrocarbon cuts or non-petroleum fillers such as pyrolysis oil.
  • the heavy hydrocarbon feedstock according to the invention may represent at least 50%, preferably 70%, more preferably at least 80%, and even more preferably at least 90% by weight of the total hydrocarbon feedstock treated by the process according to the invention.
  • the process according to the invention therefore comprises a first step a) of fixed bed hydrotreatment, optionally a step b) of separating the effluent from step a) of hydrotreatment into a light fraction and a heavy fraction, followed by a step c) bubbling bed hydrocracking of at least a portion of the effluent from step a) or at least a portion of the heavy fraction from step b), a step d) of separating the effluent from step c) to obtain at least one gaseous fraction and at least one heavy liquid fraction and finally a curing step e) and a separation step f) carried out on the heavy liquid fraction making it possible to obtain a liquid hydrocarbon fraction having a sediment content after aging less than or equal to 0.1% by weight.
  • the objective of hydrotreating is both to refine, that is to say to significantly reduce the content of metals, sulfur and other impurities, while improving the hydrogen to carbon ratio (H / C) and while transforming the hydrocarbon feed more or less partially into lighter cuts.
  • the effluent obtained in the fixed bed hydrotreating step a) can then be sent to the bubbling bed hydrocracking step c) either directly or after being subjected to a light fraction separation step.
  • Step c) allows a partial conversion of the feedstock to produce an effluent comprising in particular catalyst fines and sediments which must be removed to satisfy a product quality such as bunker oil.
  • the process according to the invention is characterized by the fact that it comprises a maturation step e) and a separation step f) carried out under conditions making it possible to improve the sediment separation efficiency and thus to obtain fuel oils. or oil bases having a sediment content after aging less than or equal to 0.1% by weight.
  • the filler according to the invention is subjected according to the process of the present invention to a fixed bed hydrotreating step a) in which the filler and hydrogen are contacted on a hydrotreatment catalyst.
  • Hydrotreatment commonly known as HDT
  • HDT Hydrotreatment
  • hydrodesulfurization reactions commonly referred to as HDS
  • hydrodenitrogenation reactions commonly referred to as HDN
  • hydrodemetallation reactions commonly referred to as HDM
  • the hydrotreatment stage a) comprises a hydrodemetallation first stage (1) (HDM) carried out in one or more hydrodemetallation zones in fixed beds and a second hydrodesulphurization second stage (a2) (HDS). performed in one or more hydrodesulfurization zones in fixed beds.
  • first step a1) of hydrodemetallation the feedstock and hydrogen are brought into contact on a hydrodemetallization catalyst, under hydrodemetallation conditions, and then during said second hydrodesulfurization step a2), the effluent of the first hydrodemetallation step a1) is brought into contact with a hydrodesulphurization catalyst, in hydrodesulfurization conditions.
  • This process known as HYVAHL-FTM, is for example described in the patent US 5417846 .
  • hydrodemetallization step hydrodemetallation reactions are carried out but also a part of the other hydrotreatment reactions and in particular hydrodesulfurization reactions.
  • hydrodesulphurization step hydrodesulphurization reactions are carried out, but also part of the other hydrotreatment reactions and in particular hydrodemetallation reactions.
  • the hydrodemetallization step begins where the hydrotreatment step begins, where the metal concentration is maximum.
  • the hydrodesulfurization step ends where the hydrotreating step ends, where sulfur removal is the most difficult.
  • the skilled person sometimes defines a transition zone in which all types of hydrotreatment reaction occur.
  • the hydrotreating step a) according to the invention is carried out under hydrotreatment conditions. It may advantageously be carried out at a temperature of between 300 ° C. and 500 ° C., preferably between 350 ° C. and 420 ° C. and under a hydrogen partial pressure of between 5 MPa and 35 MPa, preferably between MPa and 20 MPa. The temperature is usually adjusted according to the desired level of hydrotreatment and the duration of the targeted treatment.
  • the space velocity of the hydrocarbon feedstock can be in a range from 0.1 h -1 to 5 h -1 , preferably from 0.1 h -1 to 2 h -1 , and more preferably from 0.1 h -1 to 0.45 h -1 .
  • the amount of hydrogen mixed with the feedstock may be between 100 and 5000 normal cubic meters (Nm3) per cubic meter (m3) of liquid feed, preferably between 200 Nm3 / m3 and 2000 Nm3 / m3, and more preferably between 300 Nm3 / m3 and 1500 Nm3 / m3.
  • Step a) of hydrotreatment can be carried out industrially in one or more liquid downflow reactors.
  • the hydrotreatment catalysts used are preferably known catalysts. These may be granular catalysts comprising, on a support, at least one metal or metal compound having a hydrodehydrogenating function. These catalysts may advantageously be catalysts comprising at least one Group VIII metal, generally selected from the group consisting of nickel and cobalt, and / or at least one Group VIB metal, preferably molybdenum and / or tungsten. For example, it is possible to use a catalyst comprising from 0.5% to 10% by weight of nickel, preferably from 1% to 5% by weight of nickel (expressed as nickel oxide NiO), and from 1% to 30% by weight of nickel.
  • nickel oxide NiO nickel oxide
  • molybdenum preferably from 5% to 20% by weight of molybdenum (expressed as molybdenum oxide MoO3) on a mineral support.
  • This support may for example be chosen from the group consisting of alumina, silica, silica-aluminas, magnesia, clays and mixtures of at least two of these minerals.
  • this support may contain other doping compounds, in particular oxides selected from the group consisting of boron oxide, zirconia, ceria, titanium oxide, phosphoric anhydride and a mixture of these oxides. Most often an alumina support is used and very often a support of alumina doped with phosphorus and possibly boron.
  • the alumina used may be a gamma ( ⁇ ) or ⁇ (eta) alumina. This catalyst is most often in the form of extrudates.
  • the total content of metal oxides of groups VIB and VIII may be from 5% to 40% by weight and in general from 7% to 30% by weight and the weight ratio expressed as metal oxide between metal (or metals) of group VIB on metal (or metals) of group VIII is generally between 20 and 1, and most often between 10 and 2.
  • Catalysts that can be used in the hydrodemetallation step are, for example, indicated in the patent documents EP 0113297 , EP 0113284 , US 5221656 , US 5827421 , US 7119045 , US 5622616 and US 5089463 .
  • HDM catalysts are preferably used in the reactive reactors.
  • Catalysts that can be used in the hydrodesulfurization step are, for example, indicated in the patent documents EP 0113297 , EP 0113284 , US 6589908 , US 4818743 or US 6332976 .
  • the catalysts used in the process according to the present invention are preferably subjected to an in-situ or ex-situ sulphurization treatment.
  • step separating the effluent from step a) of hydrotreatment is optional.
  • step separating the effluent from step a) of hydrotreatment is not implemented, at least part of the effluent from step a) of hydrotreatment is introduced in the section allowing the implementation of step c) bubbling bed hydrocracking without changing chemical composition and without significant pressure loss.
  • "Significant loss of pressure” means a loss of pressure caused by a valve or expansion turbine, which could be estimated at a pressure loss of more than 10% of the total pressure. Those skilled in the art generally use these pressure losses or relaxations during the separation steps.
  • step a) of hydrotreatment When the separation step is carried out on the effluent from step a) of hydrotreatment, this is optionally supplemented by further additional separation steps, making it possible to separate at least one light fraction and at least one less a heavy fraction.
  • light fraction is meant a fraction in which at least 90% of the compounds have a boiling point below 350 ° C.
  • the light fraction obtained during the separation step b) comprises a gaseous phase and at least a light fraction of hydrocarbons of the naphtha, kerosene and / or diesel type.
  • the heavy fraction preferably comprises a vacuum distillate fraction and a vacuum residue fraction and / or an atmospheric residue fraction.
  • the separation step b) can be implemented by any method known to those skilled in the art. This method can be selected from high or low pressure separation, high or low pressure distillation, high or low pressure stripping, and combinations of these different methods that can operate at different pressures and temperatures.
  • the effluent from step a) hydrotreatment undergoes a step b) separation with decompression.
  • the separation is preferably carried out in a fractionation section which may firstly comprise a high temperature high pressure separator (HPHT), and possibly a low temperature high pressure separator (HPBT), followed optionally afterwards.
  • HPHT high temperature high pressure separator
  • HPBT low temperature high pressure separator
  • the effluent of step a) can be sent to a fractionation section, generally in an HPHT separator making it possible to obtain a light fraction and a heavy fraction containing predominantly boiling compounds at at least 350 ° C.
  • the separation is preferably not made according to a precise cutting point, it is rather like a separation of instantaneous type (or flash according to the Anglo-Saxon terminology).
  • the cutting point of the separation is advantageously between 200 and 400 ° C.
  • said heavy fraction can then be fractionated by atmospheric distillation into at least one atmospheric distillate fraction, preferably containing at least a light fraction of naphtha, kerosene and / or diesel type hydrocarbons, and an atmospheric residue fraction.
  • At least a portion of the atmospheric residue fraction can also be fractionated by vacuum distillation into a vacuum distillate fraction, preferably containing vacuum gas oil, and a vacuum residue fraction.
  • At least a portion of the vacuum residue fraction and / or the atmospheric residue fraction are advantageously sent to the hydrocracking step c).
  • Part of the vacuum residue may also be recycled in the hydrotreating step a).
  • the effluent from step a) hydrotreatment undergoes a step b) separation without decompression.
  • the effluent of the hydrotreatment step a) is sent to a fractionation section, generally in an HPHT separator, having a cutting point between 200 and 400 ° C. making it possible to obtain at least one light fraction and at least one heavy fraction.
  • the separation is preferably not made according to a precise cutting point, it is rather like a separation of the instantaneous type (or flash according to the English terminology).
  • the heavy fraction can then be directly sent to the hydrocracking step c).
  • the light fraction may undergo other separation steps.
  • it may be subjected to atmospheric distillation to obtain a gaseous fraction, at least a light fraction of liquid hydrocarbons of the naphtha, kerosene and / or diesel type and a vacuum distillate fraction, the last fraction possibly being at least part sent in step c) hydrocracking.
  • Another part of the vacuum distillate can be used as a fluxing agent for a fuel oil.
  • Another part of the vacuum distillate can be upgraded by being subjected to a hydrocracking step and / or catalytic cracking in a fluidized bed.
  • No-decompression separation provides better thermal integration and saves energy and equipment.
  • this embodiment has technical and economic advantages since it is not necessary to increase the flow pressure after separation before the subsequent hydrocracking step. Intermediate fractionation without decompression being simpler than fractionation with decompression, the investment cost is therefore advantageously reduced.
  • the gaseous fractions resulting from the separation step preferably undergo a purification treatment to recover the hydrogen and recycle it to the hydrotreatment and / or hydrocracking reactors.
  • the presence of the separation step between the hydrotreatment step a) and the hydrocracking step c) advantageously makes it possible to have two independent hydrogen circuits, one connected to the hydrotreatment, the hydrocracking, and which, if necessary, can be connected to each other.
  • the addition of hydrogen can be done at the hydrotreatment section or at the level of the hydrocracking section or at both.
  • the recycle hydrogen can supply the hydrotreatment section or the hydrocracking section or both.
  • a compressor may possibly be common to both hydrogen circuits.
  • the light fraction obtained at the end of the separation step b), which comprises hydrocarbons of the naphtha, kerosene and / or diesel or other type, in particular LPG and vacuum gas oil, can be recovered according to the methods which are well known in the art. the skilled person.
  • the products obtained can be incorporated into fuel formulations (also called “pools" fuels according to the English terminology) or undergo additional refining steps.
  • the fraction (s) naphtha, kerosene, gas oil and vacuum gas oil may be subjected to one or more treatments, for example hydrotreatment, hydrocracking, alkylation, isomerization, reforming. catalytic, catalytic cracking or thermal, to bring them separately or in mixture with the required specifications which may relate to the sulfur content, the smoke point, the octane number, cetane, and others.
  • At least a portion of the effluent from step a) of hydrotreatment or at least a portion of the heavy fraction from step b) is sent according to the process of the present invention in a step c) of hydrocracking which is carried out in at least one reactor, advantageously two reactors, containing at least one catalyst supported in a bubbling bed.
  • Said reactor can operate at an upward flow of liquid and gas.
  • the main objective of hydrocracking is to convert the heavy hydrocarbon feedstock into lighter cuts while partially refining it.
  • part of the initial hydrocarbon feedstock can be injected directly into the bubbling bed hydrocracking section c), mixed with the effluent of the hydrotreatment section a) in fixed bed or the heavy fraction from step b), without this portion of the hydrocarbon feedstock being treated in the hydrotreatment section a) in a fixed bed.
  • This embodiment can be likened to a partial short circuit of the hydrotreatment section a) in a fixed bed.
  • a co-charge may be introduced at the inlet of the hydrocracking section c) in a bubbling bed with the effluent of the hydrotreatment section a) in fixed bed or the heavy fraction resulting from step b) .
  • This co-charge can be chosen from atmospheric residues, vacuum residues from direct distillation, deasphalted oils, aromatic extracts from lubricant base production lines, hydrocarbon fractions or a mixture of hydrocarbon fractions that can be chosen.
  • the gas oil fractions including those obtained by atmospheric or vacuum distillation, such as, for example, vacuum gas oil.
  • this co-charge may be partially or totally injected into one of the reactors downstream of the first reactor.
  • the hydrogen necessary for the hydrocracking reaction may already be present in sufficient quantity in the effluent resulting from the hydrotreatment stage a) injected at the inlet of the hydrocracking section c) in a bubbling bed. However, it is preferable to provide an additional supply of hydrogen at the inlet of the hydrocracking section c). In the case where the hydrocracking section has several bubbling bed reactors, hydrogen can be injected at the inlet of each reactor.
  • the injected hydrogen may be a make-up stream and / or a recycle stream.
  • Bubbling bed technology is well known to those skilled in the art. Only the main operating conditions will be described here. Bubbling bed technologies conventionally use supported catalysts in the form of extrudates whose diameter is generally of the order of 1 millimeter or less.
  • the catalysts remain inside the reactors and are not evacuated with the products, except during the makeup and catalyst withdrawal phases necessary to maintain the catalytic activity.
  • the temperature levels can be high in order to obtain high conversions while minimizing the amounts of catalysts used.
  • the catalytic activity can be kept constant by replacing the catalyst in line. It is therefore not necessary to stop the unit to change the spent catalyst, nor to increase the reaction temperatures along the cycle to compensate for the deactivation.
  • working at constant operating conditions advantageously provides consistent yields and product qualities along the cycle.
  • the catalyst is kept agitated by a large recycling of liquid, the pressure drop on the reactor remains low and constant. Because of the attrition of the catalysts in the reactors, the products leaving the reactors may contain fine particles of catalyst.
  • the conditions of the bubbling bed hydrocracking step c) can be conventional bubbling bed hydrocracking conditions of a feedstock. hydrocarbon. It can be operated under an absolute pressure of between 2.5 MPa and 35 MPa, preferably between 5 MPa and 25 MPa, more preferably between 6 MPa and 20 MPa, and even more preferably between 11 MPa and 20 MPa at a temperature between 330 ° C and 550 ° C, preferably between 350 ° C and 500 ° C.
  • the space velocity (WH) and the hydrogen partial pressure are parameters that are set according to the characteristics of the product to be treated and the desired conversion.
  • the WH is generally in a range from 0.1 h -1 to 10 h -1 , preferably from 0.2 h -1 to 5 h -1 and more preferably from 0.2 h -1 to 1 h -1 .
  • the amount of hydrogen mixed with the feedstock is usually from 50 to 5000 normal cubic meters (Nm3) per cubic meter (m3) of liquid feed, most often from 100 Nm3 / m3 to 1500 Nm3 / m3 and preferably 200 Nm3 / m3 at 1200 Nm3 / m3.
  • a conventional granular hydrocracking catalyst comprising, on an amorphous support, at least one metal or metal compound having a hydrodehydrogenating function.
  • This catalyst may be a catalyst comprising Group VIII metals, for example nickel and / or cobalt, most often in combination with at least one Group VIB metal, for example molybdenum and / or tungsten.
  • a catalyst comprising from 0.5% to 10% by weight of nickel and preferably from 1% to 5% by weight of nickel (expressed as nickel oxide NiO) and from 1% to 30% by weight may be used.
  • molybdenum preferably from 5% to 20% by weight of molybdenum (expressed as molybdenum oxide MoO3) on an amorphous mineral support.
  • This support may for example be chosen from the group consisting of alumina, silica, silica-aluminas, magnesia, clays and mixtures of at least two of these minerals.
  • This support may also contain other compounds and for example oxides selected from the group consisting of boron oxide, zirconia, titanium oxide, phosphoric anhydride. Most often an alumina support is used and very often a support of alumina doped with phosphorus and possibly boron.
  • phosphorus pentoxide P2O5 When phosphorus pentoxide P2O5 is present, its concentration is usually less than 20% by weight and most often less than 10% by weight.
  • B2O3 boron trioxide When B2O3 boron trioxide is present, its concentration is usually less than 10% by weight.
  • the alumina used is usually an ⁇ (gamma) or ⁇ (eta) alumina.
  • This catalyst may be in the form of extrudates.
  • the total content of metal oxides of groups VI and VIII may be between 5% and 40% by weight, preferably between 7% and 30% by weight, and the weight ratio expressed as metal oxide between metal (or metals) of group VI on metal (or metals) of group VIII is between 20 and 1, preferably between 10 and 2.
  • the spent catalyst may be partly replaced by fresh catalyst, generally by withdrawing from the bottom of the reactor and introducing the fresh or new catalyst at the top of the reactor at a regular time interval, that is to say, for example by puff or continuously or almost continuously.
  • the catalyst can also be introduced from below and withdrawn from the top of the reactor. For example, fresh catalyst can be introduced every day.
  • the replacement rate of spent catalyst with fresh catalyst may be, for example, from about 0.05 kilograms to about 10 kilograms per cubic meter of charge. This withdrawal and this replacement are performed using devices allowing the continuous operation of this hydrocracking step.
  • the hydrocracking reactor usually comprises a recirculation pump for maintaining the catalyst in a bubbling bed by continuous recycling of at least a portion of the liquid withdrawn at the top of the reactor and reinjected at the bottom of the reactor. It is also possible to send the spent catalyst withdrawn from the reactor into a regeneration zone in which the carbon and the sulfur contained therein are eliminated before it is reinjected in the hydrocracking step (b).
  • the hydrocracking step c) according to the process of the invention can be carried out under the conditions of the H-OIL® process as described, for example, in the patent US 6270654 .
  • the bubbling bed hydrocracking can be carried out in a single reactor or in several reactors, preferably two, arranged in series.
  • the fact of using at least two bubbling bed reactors in series makes it possible to obtain products of better quality and with better performance.
  • the hydrocracking into two reactors makes it possible to have an improved operability with regard to the flexibility of the conditions operating and catalytic system.
  • the temperature of the second bubbling bed reactor is at least 5 ° C higher than that of the first bubbling bed reactor.
  • the pressure of the second reactor may be 0.1 MPa to 1 MPa lower than for the first reactor to allow the flow of at least a portion of the effluent from the first step without pumping is necessary.
  • the different operating conditions in terms of temperature in the two hydrocracking reactors are selected to be able to control the hydrogenation and the conversion of the feedstock into the desired products in each reactor.
  • the effluent obtained at the end of the first substep c1) can optionally be subjected to a separation step of the light fraction and the heavy fraction, and at least a portion, preferably all, of said heavy fraction can be treated in the second hydrocracking sub-step c2).
  • This separation is advantageously made in an inter-floor separator, as described for example in the patent US 6270654 , and in particular makes it possible to avoid over cracking of the light fraction in the second hydrocracking reactor.
  • the hydrocracking stage can also be done with several reactors in parallel (generally two) in the case of large capacity.
  • the hydrocracking step may thus comprise several stages in series, possibly separated from an inter-stage separator, each stage being constituted by one or more reactors in parallel.
  • the process according to the invention may furthermore comprise a step d) of separation which makes it possible to obtain at least one gaseous fraction and at least one heavy liquid fraction.
  • the effluent obtained at the end of the hydrocracking step c) comprises a liquid fraction and a gaseous fraction containing the gases, in particular H 2, H 2 S, NH 3, and C 1 -C 4 hydrocarbons.
  • This gaseous fraction can be separated from the effluent by means of separation devices well known to those skilled in the art, in particular with the aid of one or more separator tanks that can operate at different pressures and temperatures, possibly associated with steam or hydrogen stripping means and one or more distillation columns.
  • the effluent obtained at the end of the hydrocracking step c) is advantageously separated in at least one separator flask into at least one gaseous fraction and at least one heavy liquid fraction.
  • These separators may for example be high temperature high pressure separators (HPHT) and / or high temperature low pressure separators (HPBT).
  • this gaseous fraction is preferably treated in a hydrogen purification means so as to recover the hydrogen that is not consumed during the hydrotreatment and hydrocracking reactions.
  • the hydrogen purification means may be an amine wash, a membrane, a PSA type system, or a plurality of such means arranged in series.
  • the purified hydrogen can then advantageously be recycled in the process according to the invention, after possible recompression.
  • the hydrogen may be introduced at the inlet of the hydrotreatment step a) and / or at different locations during the hydrotreatment step a) and / or at the inlet of the hydrocracking step c) and / or at different locations during step c) hydrocracking.
  • the separation step d) may also comprise atmospheric distillation and / or vacuum distillation.
  • the separation step d) further comprises at least one atmospheric distillation, in which the fraction (s) liquid hydrocarbon (s) obtained after separation is (are) fractionated by atmospheric distillation into at least one atmospheric distillate fraction and at least one atmospheric residue fraction.
  • the atmospheric distillate fraction may contain commercially recoverable fuels bases (naphtha, kerosene and / or diesel), for example in the refinery for the production of motor and aviation fuels.
  • the separation step d) of the process according to the invention may advantageously also comprise at least one vacuum distillation in which the liquid hydrocarbon fraction (s) obtained (s) after separation. and / or the atmospheric residue fraction obtained after atmospheric distillation is (are) fractionated by vacuum distillation into at least one vacuum distillate fraction and at least one vacuum residue fraction.
  • the separation step d) comprises, first of all, an atmospheric distillation, in which the liquid hydrocarbon fraction (s) obtained after separation is (are) fractionated (s). ) by atmospheric distillation into at least one atmospheric distillate fraction and at least one atmospheric residue fraction, followed by vacuum distillation in which the atmospheric residue fraction obtained after atmospheric distillation is fractionated by vacuum distillation into at least one vacuum distillate fraction and at minus a fraction residue under vacuum.
  • the vacuum distillate fraction typically contains vacuum gas oil fractions.
  • At least a portion of the vacuum residue fraction can be recycled to the hydrocracking step c).
  • the heavy liquid fraction obtained at the end of the separation step d) contains organic sediments which result from hydrotreatment and hydrocracking conditions and catalyst residues.
  • Part of the sediments consist of asphaltenes precipitated under hydrotreatment and hydrocracking conditions and are analyzed as existing sediments (IP375).
  • IP375 existing sediments
  • IP390 sediments after aging
  • the process according to the invention comprises a maturation stage making it possible to improve the sediment separation efficiency and thus to obtain stable oil or fuel bases, that is to say a sediment content after aging less than or equal to 0.1% by weight.
  • the maturation step according to the invention makes it possible to form all the existing and potential sediments (by converting the potential sediments into existing sediments) so as to separate them more efficiently and thus respect the sediment content after aging (IP390) of 0.1% maximum weight.
  • the curing stage according to the invention is advantageously carried out for a residence time of between 1 and 1500 minutes, preferably between 25 and 300 minutes, more preferably between 60 and 240 minutes, at a temperature between 50 and 350 ° C, preferably between 75 and 300 ° C and more preferably between 100 and 250 ° C, a pressure of less than 20 MPa, preferably less than 10 MPa, more preferably less than 3 MPa and even more preferably less than 1.5 MPa.
  • the ripening step may be carried out using an exchanger or a heating furnace followed by one or more capacity (s) in series or in parallel such (s) as a horizontal or vertical balloon, optionally with a settling function to remove some of the heavier solids, and / or a piston reactor.
  • capacity s
  • a stirred and heated tank may also be used, and may be provided with a bottom draw to remove some of the heavier solids.
  • step e) of maturation of the heavy liquid fraction resulting from step d) is carried out in the presence of an inert gas and / or an oxidizing gas.
  • the aging step e) can be carried out in the presence of an inert gas such as nitrogen, or in the presence of an oxidizing gas such as oxygen, or in the presence of a mixture containing an inert gas and a oxidizing gas such as air or air depleted by nitrogen.
  • an oxidizing gas accelerates the maturation process.
  • the maturation stage is carried out in the presence of an inert and / or oxidizing gas
  • said gas is mixed with the heavy liquid fraction resulting from stage d) before the stage of maturation then separation of this gas after maturation so as to obtain a liquid fraction at the end of the stage e) of maturation.
  • a gas / liquid implementation can for example be carried out in a bubble column.
  • the inert and / or oxidizing gas may also be introduced during the maturation step e), for example by means of bubbling (injection of gas from below) into a stirred tank which allows to promote gas / liquid contact.
  • the method according to the invention further comprises a step f) of separating sediments and catalyst residues to obtain a liquid hydrocarbon fraction having a sediment content after aging less than or equal to 0.1% by weight.
  • the heavy liquid fraction obtained at the end of the maturation step e) contains precipitated asphaltene-type organic sediments which result from the hydrocracking and maturation conditions. This heavy fraction may also contain fines catalysts resulting from the attrition of extruded type catalysts in the implementation of hydrocracking reactor.
  • At least a part of the heavy liquid fraction resulting from the maturation stage e) is subjected to a separation of the sediments and the catalyst residues, by means of at least one physical separation means chosen from a filter, a separation membrane, a bed of organic or inorganic type filtering solids, electrostatic precipitation, a centrifugation system, decantation, auger withdrawal.
  • a combination, in series and / or in parallel, of several separation means of the same type or different type can be used during this step f) separation of sediments and catalyst residues.
  • One of these solid-liquid separation techniques may require the periodic use of a light rinsing fraction, resulting from the process or not, allowing for example the cleaning of a filter and the evacuation of sediments.
  • the heavy liquid fraction resulting from stage f) with a reduced sediment content may advantageously be used as a base for fuel oil or as fuel oil, in particular as a bunker oil or bunker oil base, having a sediment content after aging of less than 0. , 1% weight.
  • said heavy liquid fraction is mixed with one or more fluxing bases selected from the group consisting of catalytically cracked light cutting oils, catalytic cracked heavy cutting oils, catalytic cracking residue, a kerosene, a gas oil, a vacuum distillate and / or a decanted oil.
  • the liquid hydrocarbon fractions may, at least in part, advantageously be used as fuel oil bases or as fuel oil, especially as a bunker oil base or as a bunker oil with a sediment content after aging less than or equal to 0.1% by weight .
  • fuel oil is meant in the invention a hydrocarbon fraction that can be used as a fuel.
  • oil base is meant in the invention a hydrocarbon fraction which, mixed with other bases, is a fuel oil.
  • the liquid hydrocarbon fractions from step f) may be mixed with one or more fluxing bases selected from the group consisting of light-cutting oils of a catalytic cracking, heavy cutting oils of a catalytic cracking, the residue of a catalytic cracking, a kerosene, a gas oil, a vacuum distillate and / or a decanted oil.
  • one or more fluxing bases selected from the group consisting of light-cutting oils of a catalytic cracking, heavy cutting oils of a catalytic cracking, the residue of a catalytic cracking, a kerosene, a gas oil, a vacuum distillate and / or a decanted oil.
  • kerosene, gas oil and / or vacuum distillate produced in the process of the invention will be used.
  • the figure 1 represents a process according to the invention with separation of the effluent from the hydrotreating zone with decompression.
  • the introduction of the feedstock (10) to the outlet of the effluent (42) represents the hydrotreatment zone and this zone is described briefly because it can know many variants known to those skilled in the art.
  • the effluent leaving the at least one guard reactor (Ra, Rb) is optionally re-mixed with hydrogen arriving via line (65) in an HDM reactor (32) containing a fixed bed of catalyst.
  • an HDM reactor (32) containing a fixed bed of catalyst For readability reasons, a single HDM reactor (32) and a single HDS reactor (38) are shown in the figure, but the HDM and HDS section may include multiple HDM and HDM reactors. 'HDS in series.
  • the effluent from the HDM reactor is withdrawn through line (34) and sent to the first HDS reactor (38) where it passes through a fixed bed of catalyst.
  • the effluent from the hydrotreatment stage can be sent via line (42) into a high temperature high pressure separator (HPHT) (44) from which a gaseous fraction (46) and a liquid fraction (48) are recovered. ).
  • HPHT high temperature high pressure separator
  • the gaseous fraction (46) is sent, generally via an exchanger (not shown) or an air cooler (50) for cooling to a low temperature high pressure separator (HPBT) (52) from which a gaseous fraction (54) containing gases (H2, H2S, NH3, C1-C4 hydrocarbons, ...) and a liquid fraction (56).
  • the gaseous fraction (54) from the low temperature high pressure separator (HPBT) (52) can be treated in a hydrogen purification unit (58) from which hydrogen (60) is recovered for recycling via the compressor (62) and the line (65) to the reactors (32) and / or (38) or via the line (14) to the permutable reactors (Ra, Rb).
  • the liquid fraction (56) from the low temperature high pressure separator (HPBT) (52) is expanded in the device (68) and sent to the fractionation system (70).
  • the liquid fraction (48) from the high temperature high pressure separator (HPHT) (44) is advantageously expanded in the device (72) and then sent to the fractionation system (70). Fractions (56) and (48) can be sent together, after expansion, to the fractionation (70).
  • the fractionation system (70) advantageously comprises an atmospheric distillation system for producing a gaseous effluent (74), at least one so-called light fraction (76) and containing in particular naphtha, kerosene and diesel and an atmospheric residue fraction (78). ).
  • Part of the atmospheric residue fraction can be sent via the line (80) into the hydrocracking reactors (98, 102). All or part of the atmospheric residue fraction (78) is sent to a vacuum distillation column (82) to recover a fraction (84) containing the vacuum residue and a vacuum distillate fraction (86) containing vacuum gas oil.
  • the vacuum residue fraction (84), optionally mixed with a portion of the atmospheric residue fraction (80) and / or with a portion of the vacuum distillate fraction (86), is mixed with optionally recycled hydrogen (88). supplemented with makeup hydrogen (90) preheated in the furnace (91). It optionally passes through an oven (92).
  • a co-charge (94) may be introduced.
  • the heavy fraction is then introduced via the line (96) in the hydrocracking step at the bottom of the first bubbling bed reactor operating at an upflow of liquid and gas and containing a supported hydrocracking catalyst.
  • the converted effluent (104) from the reactor (98) may be separated from the light fraction (106) in an inter-stage separator (108).
  • All or part of the effluent (110) from the inter-stage separator (108) is advantageously mixed with additional hydrogen (157), if necessary preheated (not shown).
  • This mixture is then injected by the pipe (112) into a second hydrocracking reactor (102) also in a bubbling bed operating with an upward flow of liquid and gas containing a hydrocracking catalyst of the supported type.
  • the operating conditions, in particular the temperature, in this reactor are chosen to reach the desired conversion level, as previously described.
  • the hydrocracking reactor effluent is fed through line (134) into a high temperature high pressure (HPHT) separator (136) from which a gaseous fraction (138) and a heavy liquid fraction (140) are recovered.
  • HPHT high temperature high pressure
  • the gaseous fraction (138) is sent generally via an exchanger (not shown) or a dry cooler (142) for cooling to a low temperature high pressure separator (HPBT) (144) from which a gaseous fraction (146) containing the gaseous fraction (146) is recovered.
  • gas H2, H2S, NH3, C1-C4 hydrocarbons Certainly and a liquid fraction (148).
  • the gaseous fraction (146) of the low temperature high pressure separator (HPBT) (144) is advantageously treated in the hydrogen purification unit (150) from which hydrogen (152) is recovered for recycling via the compressor (154) and line (156) and / or line (157) to the hydrocracking section.
  • the liquid fraction (148) of the low temperature high pressure separator (HPBT) (144) is expanded in the device (160) and sent to the fractionation system (172).
  • a medium pressure separator after the expander (160) can be installed to recover a vapor phase that is sent to the purification unit (150) and / or a dedicated medium pressure purification unit (not shown). ), and a liquid phase which is fed to the fractionation section (172).
  • the heavy liquid fraction (140) from the high temperature high pressure separation (HPHT) (136) is expanded in the device (174) and sent to the fractionation system (172).
  • a medium pressure separator (not shown) after the expander (174) can be installed to recover a vapor phase that is sent to the purification unit (150) and / or a dedicated medium pressure purification unit (not shown ), and a liquid phase which is fed to the fractionation section (172).
  • Fractions (148) and (140) may be sent together, after expansion, to the system (172).
  • the fractionation system (172) comprises an atmospheric distillation system for producing a gaseous effluent (176), at least a so-called light fraction (178), containing in particular naphtha, kerosene and diesel, and an atmospheric residue fraction (180). ).
  • All or part of the atmospheric residue fraction (180) can be sent to a vacuum distillation column (184) to recover a fraction containing the vacuum residue (186) and a vacuum distillate fraction (188) containing vacuum gas oil .
  • the atmospheric residue fraction (182) and / or the vacuum residue fraction (186) are subjected to a stage of maturation and separation of sediments and catalyst residues in order to constitute desired oil bases.
  • An atmospheric residue (182) fraction is optionally preheated in an oven or exchanger (205) to achieve the temperature necessary for maturation (conversion of potential sediments into existing sediments) that occurs in the capacity (207).
  • the purpose of the capacity (207) is to provide a residence time necessary for maturation, it can therefore be a horizontal or vertical flask, a buffer tank, a stirred tank or a reactor piston.
  • the heating function can be integrated with the capacity in the case of a stirred stirred tank according to an embodiment not shown.
  • the capacity (207) may also allow settling so as to evacuate a portion of the solids (208).
  • the maturing stream (209) is then subjected to solid-liquid separation (191) to obtain a sediment-reduced fraction (212) and a sediment-rich fraction (211).
  • a vacuum residue type fraction (186) is optionally preheated in an oven or exchanger (213) so as to reach the temperature necessary for the maturation that takes place in the capacity (215).
  • the purpose of the capacity (215) is to provide a residence time necessary for maturation, it can therefore be a horizontal or vertical flask, a buffer tank, a stirred tank or a reactor piston.
  • the heating function can be integrated into the capacity in the case of a tank agitated heated according to an embodiment not shown.
  • the capacity (215) may also allow settling so as to evacuate a portion of the solids (216).
  • the maturation stream (217) is then subjected to a solid-liquid separation (192) to obtain a sediment-reduced fraction (219) and a sediment-rich fraction (218).
  • the curing devices (207) and (215) can operate in the presence of a gas, in particular an inert or oxidizing gas, or a mixture of inert gas and oxidizing gas.
  • a gas in particular an inert or oxidizing gas, or a mixture of inert gas and oxidizing gas.
  • a device not shown will separate the gas from the liquid.
  • An advantageous mode not shown may consist in operating the stage of maturation and separation of the sediments on the stream recovered at the bottom of a stripping column. When the stage of maturation and separation of sediments and catalyst residues is operated upstream of a distillation column, this column is less prone to fouling.
  • At least a portion of the streams (188) and / or (212) and / or (219) constitutes one or more desired oil bases, in particular bases for low-sulfur and low-sediment bunker fuels.
  • Part of the streams (188) and / or (212) and / or (219), before or after the sediment ripening and separation step, can be recycled via line (190) to the hydrocracking step or upstream of the hydrotreating step (line not shown).
  • the recycling of a vacuum-type gas oil section (188) upstream of the hydrotreatment can make it possible to lower the viscosity of the charge and thus facilitate pumping. Recycling an atmospheric residue type (212) or vacuum residue type (219) cutoff upstream of the hydrotreatment or hydrocracking may make it possible to increase the overall conversion.
  • the figure 2 represents another process according to the invention with separation of the effluent from the zone of hydrotreatment without decompression. It will be described below essentially only the differences between the process according to the figure 2 and the method according to figure 1 the hydrotreating, hydrocracking and separation stages after hydrocracking (and their reference signs) being moreover strictly identical.
  • the effluent treated in the hydrotreatment reactors is sent via line (42) into a high temperature high pressure separator (HPHT) (44) from which a lighter fraction (46) and a residual fraction (48) are recovered. .
  • HPHT high temperature high pressure separator
  • the residual fraction (48) is sent directly after a possible passage through an oven (92) in the hydrocracking section.
  • the lighter fraction (46) is sent, generally via an exchanger (not shown) or an air cooler (50) for cooling to a low temperature high pressure separator (HPBT) (52) from which a gaseous fraction is recovered (54). containing the gases (H2, H2S, NH3, C1-C4 hydrocarbons ...) and a liquid fraction (56).
  • HPBT high pressure separator
  • the gaseous fraction (54) of the low temperature high pressure separator (HPBT) (52) is treated in the hydrogen purification unit (58) from which hydrogen (60) is recovered for recycling via the compressor. (154) and lines (64) and (156) to the hydrotreatment section and / or the hydrocracking section.
  • Gases containing undesirable nitrogen, sulfur and oxygen compounds are advantageously removed from the plant (stream (66)).
  • a single compressor (154) is used to supply all the reactors requiring hydrogen.
  • the liquid fraction (56) from the low temperature high pressure separator (HPBT) (52) is expanded in the device (68) and sent to the fractionation system (70).
  • the fractionation system (70) comprises an atmospheric distillation system for producing a gaseous effluent (74), at least a so-called light fraction (76) and containing in particular naphtha, kerosene and diesel and an atmospheric residue fraction (195). .
  • Part of the atmospheric residue fraction can be sent, by means of a pump, not represented, via the line (195) in the hydrocracking reactors (98, 102), whereas another part of the atmospheric residue fraction ( 194) can be sent to another process (hydrocracking or FCC or hydrotreatment).
  • a variant not shown but close to the diagram of the figure 2 may consist of not using a fractionation system (70) nor to relax the liquid fraction (56) from the cold separator (52).
  • the liquid fraction (56) is then sent to the hydrocracking section optionally by means of a pump mixed with the heavy fraction (48) issuing from the separator (44).
  • the figure 3 represents another process according to the invention without a step of separation of the hydrotreatment effluent. It will be described below essentially only the differences between the process according to the figure 3 and the processes according to figures 1 and 2 the hydrotreating, hydrocracking and separation stages after hydrocracking (and their reference signs) being moreover strictly identical.
  • the effluent (42) from the fixed bed hydrotreatment reactor (38) is injected without separation and without decompression into the hydrocracking reactor (98). , via optional thermal equipment (43), (92) for adjusting the inlet temperature of the hydrocracking reactor.
  • a hydrogen-rich gas is recovered and recycled to the hydrotreating section and the hydrocracking section.
  • the feedstock was subjected to a hydrotreatment step including two permutable reactors.
  • the operating conditions are given in Table 1.
  • Table 1 Operating conditions fixed bed step of hydrotreatment ⁇ / u> HDM and HDS catalysts NiMo on alumina Temperature (° C) 370 H2 partial pressure (MPa) 15 VVH (h-1, Sm3 / h fresh load / m3 fixed bed catalyst) 0.18 H2 / HC inlet section fixed bed excluding H2 consumption (Nm3 / m3 fresh load) 1000
  • the effluent from the hydrotreatment is then subjected to a separation step making it possible to recover a light fraction (gas) and a heavy fraction containing a majority of compounds boiling at more than 350 ° C (350 ° C + fraction).
  • the heavy fraction (350 ° C + fraction) is then treated in a hydrocracking step comprising two successive bubbling bed reactors with two sets of temperatures.
  • the operating conditions of the hydrocracking step coupled with the different treatment variants (separation of sediments with or without a maturation stage) of the heavy liquid fraction resulting from atmospheric distillation have an impact on the stability of the effluents obtained. This is illustrated by the levels in post-aging sediment measured in atmospheric residues (350 ° C + cut) after the sediment separation step.
  • the stage of maturation prior to the separation of the sediments makes it possible to form all the potential sediments and thus allow their effective separation. Without maturation, beyond a certain conversion level that leads to many potential sediments, the sediment separation step is not efficient enough for the sediment content after aging (IP390) to be lower than 0.1% by weight, the maximum level required for bunker fuels.

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  • Chemical Kinetics & Catalysis (AREA)
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Claims (8)

  1. Verfahren zur Behandlung einer Kohlenwasserstoffbeschickung, die mindestens eine Kohlenwasserstofffraktion enthält, die einen Schwefelgehalt von mindestens 0,1 Gew.-%, eine anfängliche Siedetemperatur von mindestens 340 °C und eine endgültige Siedetemperatur von mindestens 440 °C aufweist, das ermöglicht, eine flüssige Kohlenwa sserstofffraktion zu erhalten, die ein Sedimentgehalt nach dem Altern von weniger als oder gleich 0,1 Gew.-% aufweist, wobei das Verfahren die folgenden Schritte aufweist:
    a) einen Schritt der Hydrobehandlung im Festbett, wobei die Kohlenwasserstoffbeschickung und der Wasserstoff über einem Hydrobehandlungskatalysator in Kontakt gebracht werden,
    b) einen optionalen Schritt des Trennens des Abstroms, der aus dem Schritt a) der Hydrobehandlung hervorgegangen ist, in mindestens eine leichte Kohlenwasserstofffraktion, die Kraftstoffgrundstoffe enthält, und in eine schwere Fraktion, die Zusammensetzungen enthält, die bei mindestens 350 °C sieden,
    c) einen Schritt des Hydrocrackens von mindestens einem Teil des Abstroms, der aus dem Schritt a) hervorgegangen ist, oder von mindestens einem Teil der schweren Fraktion, die aus dem Schritt b) hervorgegangen ist, in mindestens einem Reaktor, der einen Katalysator enthält, der im Siedebett getragen wird,
    d) einen Schritt des Trennens des Abstroms, der aus dem Schritt c) hervorgegangen ist, um mindestens eine gasförmige Fraktion und mindestens eine schwere flüssige Fraktion zu erhalten,
    e) einen Schritt des Reifens der schweren flüssigen Fraktion, die aus dem Schritt d) des Trennens hervorgegangen ist, der das Umwandeln eines Teils der potentiellen Sedimente in reale Sedimente ermöglicht, der während einer Zeitdauer zwischen 1 und 1.500 Minuten bei einer Temperatur zwischen 50 und 350 °C und mit einem Druck von unter 20 MPa durchgeführt wird,
    f) einen Schritt des Trennens der Sedimente der schweren flüssigen Fraktion, die aus dem Schritt e) des Reifens hervorgegangen ist, um eine flüssige Kohlenwasserstofffraktion zu erhalten, die einen Gehalt an Sedimenten nach dem Altern von weniger als oder gleich 0,1 Gew.-% aufweist.
  2. Verfahren nach Anspruch 1, wobei der Schritt a) der Hydrobehandlung einen ersten Schritt a1) der Hydrodemetallierung, der in einem oder mehreren Bereichen zur Hydrodemetallierung in Festbetten durchgeführt wird, und einen anschließenden zweiten Schritt a2) der Hydrodesulfurierung aufweist, der in einem oder mehreren Bereichen zur Hydrodesulfurierung in Festbetten durchgeführt wird.
  3. Verfahren nach einem der Ansprüche 1 und 2, wobei der Schritt der Hydrobehandlung a)bei einer Temperatur zwischen 300 °C und 500 °C, unter einem Wasserstoffpartialdruck zwischen 5 MPa und 35 MPa mit einer Raumgeschwindigkeit der Kohlenwasserstoffbeschickung durchgeführt wird, die in einem Bereich von 0,1 h-1 bis 5 h-1 liegt, und die Menge an Wasserstoff, die mit der Beschickung vermischt wird, zwischen 100 Nm3/m3 und 5.000 Nm3/m3 liegt.
  4. Verfahren nach einem der Ansprüche 1 bis 3, wobei der Schritt des Hydrocrackens c) unter einem absoluten Druck zwischen 5 MPa und 35 MPa, bei einer Temperatur zwischen 330 °C und 550 °C, mit einer Raumgeschwindigkeit durchgeführt wird, die in einem Bereich von 0,1 h-1 bis 10 h-1 liegt, und die Menge an Wasserstoff, die mit der Beschickung vermischt wird, 50 Nm3/m3 bis 5.000 Nm3/m3 beträgt.
  5. Verfahren nach einem der vorhergehenden Ansprüche, wobei der Schritt des Reifens der schweren flüssigen Fraktion, die aus dem Schritt d) hervorgegangen ist, in Anwesenheit eines Inertgases und/oder eines oxidierenden Gases durchgeführt wird.
  6. Verfahren nach einem der vorhergehenden Ansprüche, wobei der Schritt f) des Trennens durch mindestens ein Trennmittel durchgeführt wird, das ausgewählt wird aus einem Filter, einer Trennmembran, einem Feststofffilterbett vom organischen oder anorganischen Typ, einer elektrostatischen Ausfällung, einem Zentrifugationssystem, einer Dekantierung, einer Entnahme durch Endlosschnecke.
  7. Verfahren nach einem der vorhergehenden Ansprüche, wobei die behandelte Beschickung ausgewählt wird aus den atmosphärischen Rückständen, den Vakuumrückstanden, die aus der direkten Destillation hervorgegangen sind, Rohölen, entgasten Rohölen, den entasphaltierten Ölen, entasphaltierten Harzen, den Asphalten oder Entasphaltierungspechen, den Rückständen, die aus den Umwandlungsverfahren von aromatischen Extrakten hervorgegangen sind, die aus den Produktionsketten von Basen für Schmiermittel stammen, Teersanden oder deren Derivaten, Ölschiefern oder deren Derivaten, allein genommen oder im Gemisch.
  8. Verfahren nach einem der vorhergehenden Ansprüche, wobei die flüssigen Kohlenwasserstofffraktionen, die aus dem Schritt f) hervorgegangen sind, mit einer oder mehreren verdünnenden Grundstoffen vermischt werden, die ausgewählt werden aus der Gruppe, bestehend aus den Ölen einer leichten Fraktion eines katalytischen Crackens, den Ölen einer schweren Fraktion eines katalytischen Crackens, dem Rest eines katalytischen Crackens, einem Kerosin, einem Dieselöl, einem Vakuumdestillat und/oder einem dekantierten Öl.
EP15306717.8A 2014-11-04 2015-10-27 Verfahren zur umwandlung von erdöleinsätzen, das eine hydrotreating-phase im festbett, eine hydrocracking-phase in einer wirbelschicht, eine reifephase und eine abscheidungsphase von sedimenten für die herstellung von heizöl mit geringem sedimentanteil umfasst Active EP3018188B1 (de)

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CN105567314A (zh) 2016-05-11
KR102447843B1 (ko) 2022-09-26
US20160122665A1 (en) 2016-05-05
CN105567314B (zh) 2019-08-06
KR20160052444A (ko) 2016-05-12
FR3027910A1 (fr) 2016-05-06
EP3018188A1 (de) 2016-05-11
FR3027910B1 (fr) 2016-12-09
US9834731B2 (en) 2017-12-05
ES2656417T3 (es) 2018-02-27

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