EP0354623B1 - Procédé d'hydrocraquage de charges hydrocarbonées - Google Patents

Procédé d'hydrocraquage de charges hydrocarbonées Download PDF

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Publication number
EP0354623B1
EP0354623B1 EP19890202059 EP89202059A EP0354623B1 EP 0354623 B1 EP0354623 B1 EP 0354623B1 EP 19890202059 EP19890202059 EP 19890202059 EP 89202059 A EP89202059 A EP 89202059A EP 0354623 B1 EP0354623 B1 EP 0354623B1
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EP
European Patent Office
Prior art keywords
effluent
process according
reaction stage
hydrocracking
hydrogen
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP19890202059
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German (de)
English (en)
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EP0354623A1 (fr
Inventor
Kees Jan Willem Groeneveld
Antoine Sarkis Hanna
Swan Tiong Sie
Oscar Sy
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Shell Internationale Research Maatschappij BV
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Shell Internationale Research Maatschappij BV
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Publication date
Priority claimed from GB888819122A external-priority patent/GB8819122D0/en
Priority claimed from CA000604067A external-priority patent/CA1320925C/fr
Application filed by Shell Internationale Research Maatschappij BV filed Critical Shell Internationale Research Maatschappij BV
Publication of EP0354623A1 publication Critical patent/EP0354623A1/fr
Application granted granted Critical
Publication of EP0354623B1 publication Critical patent/EP0354623B1/fr
Expired legal-status Critical Current

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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
    • 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
    • C10G65/10—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including only cracking steps

Definitions

  • the present invention relates to a process for the hydrocracking of a hydrocarbonaceous feedstock in which a plurality of reaction stages are employed.
  • Hydrocracking is a well-established process in which heavy hydrocarbons are contacted in the presence of hydrogen with a hydrocracking catalyst.
  • the temperature and the pressure are relatively high, so that the heavy hydrocarbons are cracked to products with a lower boiling point.
  • the process can be carried out in one stage, it has shown to be advantageous to carry out the process in a plurality of stages. In a first stage the feedstock is subjected to denitrogenation, desulphurisation and hydrocracking, and in a second stage most of the hydrocracking reactions occur.
  • the presence of nitrogen compounds in the feedstock may lead to problems as, generally, hydrocracking catalysts are nitrogen-sensitive and may be deactivated by the nitrogen compounds. Therefore it has been proposed to remove the nitrogen compounds from the effluent of the first stage.
  • the nitrogen compounds usually comprising ammonia, may be washed out by subjecting the first stage effluent to a treatment with an aqueous solution of, for example, a mineral acid.
  • an aqueous solution of, for example, a mineral acid Apart from the fact that the washing procedure does not always remove any organic nitrogen compounds that remain in the effluent, there is the drawback that the effluent needs to be cooled off significantly in order to obtain a satisfactory removal of the ammonia.
  • Another drawback of the above procedure resides in the fact that hydrocarbonaceous products that have already been cracked and are valuable desired products, remain in the effluent and can again be cracked in the second stage to yield less desired lighter or even undesired gaseous products.
  • a petroleum purification process which comprises firstly subjecting a petroleum material to a hydrodesulphurization treatment, and subsequently subjecting the liquid bottom fraction obtained therefrom to a non-catalytic hydrocracking step.
  • the present invention provides a process for the hydrocracking of a hydrocarbonaceous feedstock which process comprises contacting the feedstock in a first reaction stage at a temperature from 320 to 450 °C and a pressure from 50 to 250 bar in the presence of hydrogen with a first hydrocracking catalyst to obtain a first effluent, separating from the first effluent a gaseous phase and a liquid phase at substantially the same temperature and pressure as prevailing in the first reaction stage, contacting the liquid phase of the first effluent in a second reaction stage at a temperature from 300 to 450 °C and a pressure from 50 to 250 bar in the presence of hydrogen with a second hydrocracking catalyst to obtain a second effluent and obtaining at least one desired product by fractionation of the combined gaseous phase and second effluent.
  • At least one distillate fraction and a residual fraction are obtained by fractionation, and at least a part of the residual fraction is recycled to a reaction stage.
  • the complete residual fraction It is preferred to recycle the complete residual fraction. This has the advantage that the complete feedstock is hydrocracked to products with a lower boiling point. This part or the complete residual fraction may be recycled to the first reaction stage. However, since the residual fraction is substantially nitrogen-free and since most of the hydrocracking reactions occur in the second reaction stage, it is preferred to pass the (part of the) residual fraction to the second reaction stage. Thereto it is convenient to combine it with the liquid phase of the first effluent before it is passed to the second reaction stage.
  • the desired product or products are obtained by fractionation without recycle.
  • the gaseous phase of the first effluent contains hydrogen and ammonia and generally hydrogen sulphide, and the second effluent comprises at least hydrogen. It is preferred to remove the ammonia and the hydrogen sulphide from the process and to recover the hydrogen which can be recycled to the hydrocracking reactors. Therefore, preferably the gaseous phase of the first effluent and the second effluent are subjected to a removal step of ammonia and hydrogen before being subjected to fractionation.
  • the procedures for the removal of hydrogen, ammonia (and hydrogen sulphide) are known in the art and do not need to be described here.
  • Hydrocarbonaceous feedstocks that can be used in the present process include gas oils, vacuum gas oils, deasphalted oils, long residues, short residues, catalytically cracked cycle oils, thermally cracked gas oils and syncrudes, optionally originating from tar sands, shale oils, residue upgrading processes or biomass. Combinations of various hydrocarbonaceous feedstock can also be employed. Th hydrocarbonaceous feedstock will generally be such that a major part, say over 50 %wt, has a boiling point above 370 °C. The present process is most advantageous when the feedstock contains nitrogen. Typical nitrogen contents are in the range of up to 5000 ppmw. Nitrogen contents may start from 50 ppmw. The feedstock will generally also comprise sulphur compounds. The sulphur content will usually be in the range from 0.1 to 6 %wt.
  • the separation of a gaseous and a liquid phase of the first effluent takes place at substantially the same temperature and pressure as prevailing in the first reaction stage. Conveniently this is achieved by refraining from cooling or heating the first effluent.
  • the effluent is passed to a separate separation vessel, suitably a high temperature, high pressure interstage flash vessel arranged at or near the outlet of the first reaction stage.
  • this separation vessel may consist of any suitable device known in the art for the separation of a gas and a liquid.
  • the separation vessel is a settling vessel from which at a lower portion the liquid is withdrawn and from an opening above the liquid level the gas is withdrawn.
  • the first reaction stage and the separation are carried out in the same reaction vessel. This can be achieved by the creation of a settling area in the bottom part of the reaction vessel, from which the gaseous phase and the liquid phase are withdrawn via different openings. This embodiment entails the advantage that no separate separation vessel is needed.
  • the temperature and the pressure of the separation are substantially the same as those prevailing in the first reaction stage. It will be appreciated that minor fluctuations in the reaction conditions in the first reaction stage may occur.
  • the temperature and the pressure in the separation are then preferably substantially the same as those prevailing in the exit part of the first reaction zone. These conditions include a temperature of 320 to 450 °C and a pressure of 50 to 250 bar. Preferably, the temperature is from 375 to 425 °C and the pressure is from 75 to 150 bar.
  • the temperature and pressure are preferably from 375 to 425 °C and 75 to 150 bar.
  • the hydrogen/oil ratio in the first reaction stage is suitably from 500 to 5000 Nl/kg, more preferably from 750 to 2500 Nl/kg, and the space velocity from 0.1 to 10 kg/l/h, more preferably from 0.2 to 5 kg/l/h.
  • the catalyst in the first stage is preferably a hydrocracking catalyst which also has hydrodenitrogenation activity.
  • Suitable catalysts include a refractory oxide in combination with a group 8 and/or group 6b metal or component thereof.
  • Suitable refractory oxides include alumina, silica, silica-alumina, magnesia, titania, zirconia and clays.
  • the catalyst is a alumina-based catalyst with a group 8 and/or group 6b metal or component thereof.
  • the catalytically active metal from groups 8 and 6b are preferably selected from cobalt, nickel, platinum, palladium, tungsten and molybdenum.
  • Preferably non-noble metal mixtures are used, such as Ni-W, Ni-Mo, Co-Mo and Co-W.
  • the catalyst may further contain phosphorus and/or fluorine to boost its activity.
  • the catalytically active metals are non-noble they are preferably present on the first hydrocracking catalyst in an amount of 1 to 16 %wt of a group 8 metal and/or from 6 to 24 %wt of a group 6b metal, the weight percentages being based on the total catalyst.
  • Noble metals are suitably present in a lower amount, e.g.
  • the catalytically active metals are non-noble they are preferably present in their oxidic or even more preferred in their sulphidic form.
  • the preparation of the first hydrocracking catalyst is known in the art.
  • the second hydrocracking catalyst is preferably different from the first hydrocracking catalyst.
  • the second hydrocracking catalyst may be sensitive to nitrogen compounds.
  • Suitable catalysts include hydrocracking catalysts based on silica-alumina and zeolites. Silica-alumina-based catalysts which tend to be highly nitrogen-sensitive, can be used because of the efficient ammonia removal in the interstage separation. Since zeolitic hydrocracking catalysts tend to be more active, they are especially preferred.
  • Suitable zeolitic catalysts comprise a faujasite-type zeolite, in particular zeolite Y. The silica/alumina molar ratio in such zeolites may vary from 4 to 25, in particular from 6 to 15.
  • the unit cell size of zeolite Y may vary from 2.419 to 2.475 nm, in particular from 2.425 to 2.460 nm.
  • the second hydrocracking catalyst conveniently comprises further catalytically active metals and at least one binder.
  • the binder is suitably selected from silica, alumina, thoria, titania, silica-alumina, zirconia, magnesia and mixtures thereof.
  • alumina is preferred, optionally in combination with silica-alumina.
  • the catalytically active components on the second hydrocracking catalyst are the same as those on the first hydrocracking catalyst, i.e. a group 8 and/or a group 6b metal or compound thereof.
  • Nickel, cobalt, platinum, palladium, tungsten and molybdenum are preferred.
  • the non-noble metals are preferably in their oxidic or sulphidic form.
  • the amounts of the metals are preferably from 2 to 25 %wt of a group 6b metal, from 1 to 16 %wt of a group 8 metal when the group 8 metal is not noble and from 0.2 to 2 %wt of a noble group 8 metal, all percentages being based on total catalyst.
  • the process conditions prevailing in the second reaction stage are preferably a temperature from 300 to 425 °C, a pressure from 50 to 250 bar, a space velocity from 0.1 to 10 kg/l/h, and a hydrogen/oil ratio of 250 to 5000 Nl/kg.
  • Figure 1 shows one embodiment of the present process in which use is made of a separate separation vessel.
  • FIG. 2 shows an alternative embodiment in which no separation vessel is needed.
  • a first hydrocracking reactor 1 which contains one or more catalyst beds.
  • one catalyst bed 13 is shown, comprising a first hydrocracking catalyst, e.g. an alumina-based catalyst loaded with nickel and molybdenum.
  • a hydrocarbonaceous feedstock is passed through a line 11 and mixed with a hydrogen-containing gas supplied via a line 12.
  • the mixture is passed through the catalyst bed(s) and a first effluent is withdrawn at the bottom of the first reactor via a line 14.
  • the first effluent is passed to a separation vessel 3 which operates at substantially the same temperature and pressure as used in the reactor 1.
  • a gaseous phase is separated from a liquid phase.
  • the liquid phase is withdrawn via a line 16 and is subsequently mixed with a residual fraction supplied via a line 17a.
  • the mixture is then passed to a second hydrocracking reactor 2 via the line 17 after having been mixed with a hydrogen-containing gas supplied via a line 18.
  • the second hydrocracking reactor 2 contains one or more catalyst beds, here indicated as catalyst bed 19.
  • the catalyst in the second reactor 2 is advantageously an amorphous silica-alumina carrier loaded with nickel/tungsten or nickel/molybdenum or a zeolite Y-containing carrier loaded with nickel/tungsten or nickel/molybdenum.
  • the mixture from the line 17 is hydrocracked and a second effluent is discharged via a line 20, where it is mixed with the gaseous phase of the first effluent from the line 15.
  • the resulting mixture is passed to a separation section 5 where in several stages hydrogen is recovered from the second effluent, ammonia and hydrogen sulphide that have been formed during the process are removed and a hydrocarbonaceous product is obtained.
  • the hydrogen is recovered via a line 22, where it is mixed with make-up hydrogen supplied via a line 23.
  • the line 22 then splits into the lines 12 and 18 that provide the hydrogen for the reactors 1 and 2, respectively.
  • the waste ammonia and hydrogen sulphide are discharged via a line 21 and can be subjected to gas purification and sulphur recovery.
  • the hydrocarbonaceous product is passed via a line 24 to a fractionation section, here indicated as a fractionator 4, where it is divided into gaseous and liquid distillate fractions that are recovered via lines 25, 25a, 25b and 25c.
  • the residue of the fractionation is withdrawn via the line 17a. It will be apparent that the cut point for the residual fraction can be arranged at will in accordance with the desired products.
  • line 17a recycles the residual fraction to the line 17. Recycle may not be necessary if once-through operation results in an acceptable product slate.
  • the separation vessel has been deleted.
  • the numbering of equipment in Figure 2 is the same as in Figure 1 when reference is made to corresponding equipment.
  • the hydrocarbonaceous feedstock is mixed with a hydrogen-containing gas and passed to the first hydrocracking reactor 1.
  • the reactor 1 is provided with a settling area 30.
  • a first effluent enters the settling zone 30 and a separation occurs between a gaseous and liquid phase.
  • the liquid phase is withdrawn from the reactor at the bottom of the reactor 1 via a line 32, and the gaseous phase is withdrawn from the reactor 1 at a higher position via a line 31.
  • the liquid phase in line 32 is mixed with the residual fraction from the fractionator 4 in line 17a and is subsequently cracked in the second hydrocracking reactor 2.
  • the second effluent is withdrawn via the line 20, mixed with the gaseous phase of the first effluent from line 31 and the resulting mixture is worked up as described for the embodiment of Figure 1.
  • a feedstock A derived from a synthetic crude, originating from the upgrading of Athabasca tarsands (syncrude, Fort McMurray, Canada), and having the properties given in Table 1 below, was subjected to first stage hydrotreating over a commercially available catalyst containing nickel (3% by weight), molybdenum (13% by weight) and phosphorus (3.2% by weight) on alumina, which catalyst had been diluted with an equal volume of 0.2 mm SiC and calcined and sulphided prior to use.
  • the hydrotreating was carried out at an inlet pressure of 125 bar, a space velocity of 1 kg/l/h and a hydrogen/oil ratio of 800 to 900 nl/kg.
  • the temperature was adjusted to maintain a conversion of 338 °C+ materials of 21-22% and was in the range of 380 to 383 °C.
  • the total first stage liquid products were recovered.
  • a portion of the first stage liquid product was subjected to a fractionation to produce a top and bottom fraction.
  • the bottom fraction, feedstock B had the properties given in Table 1 and was selected to represent the calculated feedstock constitution obtained by subjecting the product of the first stage hydrotreating to a gas/liquid separation at substantially the same high temperature and pressure as prevailing at the outlet of the first stage, i.e. 395 °C and 140 bar.
  • Dosages of dimethyl disulphide and t-butylamine were incorporated in feedstock B to adjust the level of H2S and NH3 to that which would be present in a liquid effluent obtained by such high temperature and pressure separation.
  • Feedstocks B and C were separately subjected to once-through hydrocracking in a second stage over a zeolitic catalyst comprising 8.4 %w W and 2.5 %w Ni.
  • the zeolitic catalyst carrier consisted of 10 %w alumina and 90 %w zeolite Y having a unit cell size of 2.433 nm.
  • the catalyst was diluted with an equal volume of 0.2 mm SiC, calcined and sulphided prior to use.
  • the hydrocracking was carried out at conditions selected to give the desired conversion of 338 °C+ materials.
  • the second stage was operated at an inlet pressure of 125 bar, a space velocity of 0.46 to 0.50 kg/l/hr, a temperature of 378 to 379 °C and a hydrogen/oil ratio of 940 to 1025 nl/kg.

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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)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Claims (12)

1. Procédé d'hydrocraquage d'une charge hydrocarbonée, qui consiste : à mettre en contact la charge dans un premier étage de réaction à une température de 320 à 450°C et sous une pression de 50 à 250 bars en présence d'hydrogène en contact avec un premier catalyseur d'hydrocraquage pour obtenir un premier effluent ; à séparer du premier effluent une phase gazeuse et une phase liquide à une température et une pression qui prédominent au premier étage de réaction ; à mettre en contact la phase liquide du premier effluent dans un second étage de réaction à une température de 300 à 450°C et sous une pression de 50 à 250 bars en présence d'hydrogène avec un second catalyseur d'hydrocraquage pour obtenir un second effluent et obtenir au moins un produit désiré par fractionnement de la phase gazeuse combinée et du second effluent.
2. Procédé selon la revendication 1, dans lequel on obtient au moins une fraction de distillat et une fraction résiduelle par fractionnement et on recycle une partie au moins de la fraction résiduelle à l'étage de réaction.
3. Procédé selon la revendication 2, dans lequel on recycle à l'étage de réaction la fraction résiduelle complète.
4. Procédé selon la revendication 2 ou 3, dans lequel on recycle la fraction résiduelle (ou une partie de celle-ci) et on la combine avec la phase liquide du premier effluent, puis on la transfère au second étage de réaction.
5. Procédé selon la revendication 1, dans lequel on obtient le ou les produit(s) désiré(s) sans recyclage.
6. Procédé selon l'une quelconque des revendications 1 à 5, dans lequel on soumet la phase gazeuse du premier effluent et du second effluent à un stade de soutirage d'ammoniac et d'hydrogène avant le fractionnement.
7. Procédé selon l'une quelconque des revendications 1 à 6, dans lequel on effectue la séparation du premier effluent sans chauffer ou refroidir l'effluent.
8. Procédé selon l'une quelconque des revendications 1 à 7, dans lequel on effectue le premier étage de réaction et la séparation dans le même récipient de réaction.
9. Procédé selon l'une quelconque des revendications 1 à 8, dans lequel le rapport hydrogène/huile dans le premier étage de réaction est de 500 à 5000 Nl/kg et la vitesse spatiale est de 0,1 à 10 kg/l/h.
10. Procédé selon l'une quelconque des revendications 1 à 9, dans lequel le premier catalyseur d'hydrocraquage est un catalyseur à base d'alumine comprenant un métal du groupe 8 et/ou du groupe 6B ou un composé de celui-ci.
11. Procédé selon l'une quelconque des revendications 1 à 10, dans lequel, au second étage de réaction, la vitesse spatiale est de 0,1 à 10 kg/l/h et le rapport hydrogène/huile est de 250 à 5000 Nl/kg.
12. Procédé selon l'une quelconque des revendications 1 à 11, dans lequel le second catalyseur d'hydrocraquage est un catalyseur à base de zéolite comprenant un métal du Groupe 8 et/ou du Groupe 6B ou un composé de celui-ci.
EP19890202059 1988-08-11 1989-08-08 Procédé d'hydrocraquage de charges hydrocarbonées Expired EP0354623B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
GB888819122A GB8819122D0 (en) 1988-08-11 1988-08-11 Process for hydrocracking of hydrocarbonaceous feedstock
GB8819122 1988-08-11
CA000604067A CA1320925C (fr) 1989-06-27 1989-06-27 Procede d'hydrocraquage d'une charge d'alimentation hydrocarbonee
CA604067 1989-06-27

Publications (2)

Publication Number Publication Date
EP0354623A1 EP0354623A1 (fr) 1990-02-14
EP0354623B1 true EP0354623B1 (fr) 1992-06-03

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP19890202059 Expired EP0354623B1 (fr) 1988-08-11 1989-08-08 Procédé d'hydrocraquage de charges hydrocarbonées

Country Status (6)

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EP (1) EP0354623B1 (fr)
JP (1) JPH02153992A (fr)
AU (1) AU615565B2 (fr)
DE (1) DE68901696T2 (fr)
ES (1) ES2032103T3 (fr)
SG (1) SG45293G (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104650974B (zh) * 2013-11-20 2016-08-17 中国石油化工股份有限公司 降低轻馏分产品硫含量的加氢裂化工艺方法

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1482023B1 (fr) * 2000-11-11 2008-04-09 Haldor Topsoe A/S Procédé permettant d'adapter des réacteurs d'hydrocraquage existants
US6841062B2 (en) * 2001-06-28 2005-01-11 Chevron U.S.A. Inc. Crude oil desulfurization
US7354560B2 (en) 2006-01-31 2008-04-08 Haldor Topsoe A/S Process for the production of hydrogen
CA3037670C (fr) * 2016-09-30 2025-05-13 Hindustan Petroleum Corporation Limited Procédé de valorisation d'hydrocarbures lourds

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3365388A (en) * 1965-06-08 1968-01-23 Chevron Res Multistage residuum hydroconversion process
DE1770267A1 (de) * 1967-04-25 1971-12-23 Atlantic Richfield Co Verfahren zur Entschwefelung von Erdoelprodukten
US3554898A (en) * 1968-08-29 1971-01-12 Union Oil Co Recycle hydrocracking process for converting heavy oils to middle distillates
NL7605356A (nl) * 1975-05-21 1976-11-23 Inst Francais Du Petrole Werkwijze voor het hydrokraken van koolwater- stofolien.

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104650974B (zh) * 2013-11-20 2016-08-17 中国石油化工股份有限公司 降低轻馏分产品硫含量的加氢裂化工艺方法

Also Published As

Publication number Publication date
ES2032103T3 (es) 1993-01-01
DE68901696D1 (de) 1992-07-09
AU615565B2 (en) 1991-10-03
AU3945489A (en) 1990-02-15
JPH02153992A (ja) 1990-06-13
EP0354623A1 (fr) 1990-02-14
SG45293G (en) 1993-06-25
DE68901696T2 (de) 1992-12-17

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