EP0082551B1 - Process for the production of hydrocarbon oil distillates - Google Patents

Process for the production of hydrocarbon oil distillates Download PDF

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Publication number
EP0082551B1
EP0082551B1 EP82201560A EP82201560A EP0082551B1 EP 0082551 B1 EP0082551 B1 EP 0082551B1 EP 82201560 A EP82201560 A EP 82201560A EP 82201560 A EP82201560 A EP 82201560A EP 0082551 B1 EP0082551 B1 EP 0082551B1
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Prior art keywords
stream
feed
treatment
asphaltenes
separated
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Expired
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EP82201560A
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German (de)
English (en)
French (fr)
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EP0082551A1 (en
Inventor
Robert Hendrik Van Dongen
John Robert Newsome
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Shell Internationale Research Maatschappij BV
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Shell Internationale Research Maatschappij BV
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G67/00Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
    • C10G67/02Treatment 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
    • C10G67/04Treatment 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 including solvent extraction as the refining step in the absence of hydrogen
    • C10G67/0454Solvent desasphalting
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10Feedstock materials
    • C10G2300/107Atmospheric residues having a boiling point of at least about 538 °C

Definitions

  • the invention relates to a process for the production of hydrocarbon oil distillates from asphaltenes-containing hydrocarbon mixtures.
  • GB-A-1 560 148 a process is described wherein an atmospheric hydrocarbon oil residue is subjected to a catalytic hydrotreatment and the hydrotreated product is separated by distillation into one or more atmospheric distillates, a vacuum distillate and a vacuum residue.
  • the vacuum residue is separated by deasphalting into a deasphalted oil and asphalt.
  • the vacuum distillate and the deasphalted oil are converted by catalytic cracking and/or hydrocracking into one or more atmospheric distillates and at least 50 %w of the asphalt is again subjected to catalytic hydrotreatment.
  • the atmospheric residue may be subjected to thermal cracking. Further, the atmospheric residue may be separated by vacuum distillation into a vacuum distillate and a vacuum residue, the vacuum distillate may be subjected to thermal cracking or to catalytic cracking in the presence or in the absence of hydrogen and the vacuum residue to thermal cracking. Finally, the vacuum residue may be separated by solvent deasphalting into a deasphalted oil and an asphaltic bitumen, the deasphalted oil may be subjected to thermal cracking or to catalytic cracking in the presence or in the absence of hydrogen, and the asphaltic bitumen to thermal cracking.
  • Thermal cracking refers to a process wherein a heavy feedstock is converted into a product which contains less than 20 %w C4- hydrocarbons and from which one or more distillate fractions may be separated as the desired light product and a heavy fraction as a by-product.
  • TC has proved in actual practice to be a suitable treatment for the production of hydrocarbon oil distillates from a variety of asphaltenes-containing hydrocarbon mixtures.
  • DA solvent deasphalting
  • HT catalytic hydrotreatment
  • the deasphalted oil fraction which is separated from the product of the DA treatment is used as the feed or a feed component for the TC treatment.
  • Each of the embodiments may be placed in one of the following three classes:
  • the embodiments to which the present patent application relates may further be subdivided depending on whether the heavy fraction separated from the product from the HT is used as feed for the DA treatment (class IA), or as a feed component for the TC (class IB). In the embodiments belonging to class IB the heavy fraction separated from the TC treatment is used as feed for the DA treatment.
  • the present patent application therefore relates to a process for the production of hydrocarbon oil distillates from asphaltenes-containing hydrocarbon mixtures, in which an asphaltenes-containing hydrocarbon mixture (stream 1) is subjected to a catalytic hydrotreatment (HT) in which an asphaltenes-containing feed is converted into a product having a reduced asphaltenes content from which one or more distillate fractions and a heavy fraction (stream 2) are separated, in which stream 2 is subjected to a combination of the following two treatments: solvent deasphalting (DA) in which an asphaltenes-containing feed is converted into a product from which a deasphalted oil fraction (stream 3) and an asphaltic bitumen fraction (stream 4) are separated and thermal cracking (TC) in which one feed or two individual feeds are converted into a product which contains less than 20 %w C4- hydrocarbons and from which one or more distillate fractions and a heavy fraction (stream 5) are separated, in which stream 3 is used as the feed or as a feed component for the
  • the feed used is an asphaltenes-containing hydrocarbon mixture.
  • a suitable parameter for the assessment of the asphaltenes content of a hydrocarbon mixture as well as of the reduction of the asphaltenes content which appears when an asphaltenes-containing hydrocarbon mixture is subjected to a HT, is the Ramsbottom Carbon Test value (RCT).
  • RCT Ramsbottom Carbon Test value
  • the process is applied to hydrocarbon mixtures which boil substantially above 350°C and more than 35% w of which boils above 520°C and which have an RCT of more than 7.5% w.
  • hydrocarbon mixtures are residues obtained in the distillation of crude mineral oils and also heavy hydrocarbon mixtures obtained from shale and tar sand. If required, the process may also be applied to heavy crude mineral oils, residues obtained in the distillation of products formed in the thermal cracking of hydrocarbon mixtures and asphaltic bitumen obtained in the solvent deasphalting of asphaltenes-containing hydrocarbon mixtures.
  • the process according to the invention can very suitably be applied to residues obtained in the vacuum distillation of atmospheric distillation residues from crude mineral oils. If an atmospheric distillation residue from a crude mineral oil is available as feed for the process according to the invention, it is preferred to separate a vacuum distillate therefrom by vacuum distillation and to subject the resulting vacuum residue to the HT.
  • the separated vacuum distillate may be subjected to thermal cracking or to catalytic cracking in the presence or in the absence of hydrogen to convert it into light hydrocarbon oil distillates.
  • the separated vacuum distillate is very suitable for use as a feed component for the TC treatment, together with stream 3.
  • the process according to the invention is a three-step process in which in the first step an asphaltenes-containing feed (stream 1) is subjected to a HT for the production of a product with a reduced asphaltenes content from which one or more distillate fractions and a heavy fraction (stream 2) are separated. In the second and third steps of the process stream 2 is subjected to a combination of a DA treatment and a TC treatment.
  • Asphaltenes-containing hydrocarbon mixtures usually include a considerable percentage of metals particularly vanadium and nickel.
  • a catalytic treatment for instance a HT for the reduction of the asphaltenes content
  • these metals are deposited on the catalyst used in the HT and thus shorten its effective life.
  • asphaltenes-containing hydrocarbon mixtures having a vanadium+nickel content of more than 50 parts per million by weight (ppmw) should preferably be subjected to a demetallization treatment before they are contacted with the catalyst used in the HT.
  • This demetallization may very suitably be carried out by contacting the asphaltenes-containing hydrocarbon mixture, in the presence of hydrogen, with a catalyst consisting more than 80% w of silica.
  • a catalyst consisting more than 80% w of silica.
  • Both catalyst completely consisting of silica and catalysts containing one or more metals having hydrogenating activity-in particular a combination of nickel and vanadium-emplaced on a carrier substantially consisting of silica are suitable for the purpose.
  • the asphaltenes-containing feed is subjected to a catalytic demetallization treatment in the presence of hydrogen, this demetallization may be carried out in a separate reactor.
  • the two processes may very suitably be carried out in the same reactor containing a bed of the demetallization catalyst and a bed of the catalyst used in the HT, successively.
  • catalysts for carrying out the HT are those containing at least one metal chosen from the group formed by nickel and cobalt and in addition at least one metal chosen from the group formed by molybdenum and tungsten on a carrier, which carrier consists more than 40% w of alumina.
  • Catalysts very suitable for use in the HT are those comprising the metal combinations nickel/molybdenum or cobalt/molybdenum on alumina as the carrier.
  • the HT is preferably carried out at a temperature of from 300-500°C and in particular of from 350-450°C, a pressure of from 50-300 bar and in particular of from 75 ⁇ 200 bar, a space velocity of from 0.02 ⁇ 10 g.g.
  • the HT is preferably carried out in such a way that it yields a product the Cs fraction of which meets the following requirements:
  • the first step of the process according to the invention yields a product having a reduced asphaltenes content from which one or more distillate fractions and a heavy fraction (stream 2) are separated.
  • the distillate fractions separated from the product may be atmospheric distillates only, but it is preferred to separate a vacuum distillate from the product as well. This vacuum distillate may be converted into light hydrocarbon oil distillates in the ways stated hereinbefore.
  • the second or third step used is a DA treatment in which an asphaltenes-containing feed is converted into a product from which a deasphalted oil fraction (stream 3) and an asphaltic bitumen fraction (stream 4) are separated.
  • Suitable solvents for carrying out the DA are paraffinic hydrocarbons having of from 3-6 carbon atoms per molecule, such as n-butane and mixtures thereof, such as mixtures of propane and n-butane and mixtures of n-butane and n-pentane. Suitable solvent/oil weight ratios lie between 7:1 and 1:1 and in particular between 4:1 and 1:1.
  • the DA treatment is preferably carried out at a pressure in the range of from 20 to 100 bar.
  • the deasphalting is preferably carried out at a pressure of from 35-45 bar and a temperature of from 100-150°C.
  • the second or third step used is a TC treatment in which one feed or two separate feeds are converted into a product which contains less than 20% w C4 hydrocarbons and from which one or more distillate fractions and a heavy fraction (stream 5) are separated.
  • the way in which the TC treatment is carried out is determined by the quality of the feeds available for the TC.
  • the feed for the TC is composed of nothing but one or more streams having a relatively low asphaltenes content, such as stream 3-optionally together with one or more vacuum distillates separated during the process-a TC treatment comprising a single cracking unit will be sufficient.
  • one or more distillate fractions and a heavy fraction are separated.
  • the distillate fractions separated from the product may be atmospheric distillates only, but it is preferred to separate a vacuum distillate from the product as well. This vacuum distillate may be converted into light hydrocarbon oil distillates in the ways stated hereinbefore.
  • the feed for the TC treatment is composed of nothing but one or more streams having a relatively low asphaltenes content, and a TC treatment is used which comprises only one cracking unit, then a heavy fraction of the cracked product is preferably recirculated to the cracking unit.
  • a product may be prepared from which one or more atmospheric distillates are separated by distillation and subsequently part of the atmospheric residue may be recirculated to the cracking unit.
  • the feed for the TC treatment is composed of both of one or more streams having a relatively low asphaltenes content, such as stream 3-optionally together with one or more vacuum distillates separated during the process-and of a relatively asphaltenes-rich stream, such as stream 4 or stream 2 obtained as vacuum residue
  • a TC treatment comprising two cracking units and to crack the two feeds separately to form products from which one or more distillate fractions and a heavy fraction (stream 5) are separated.
  • the distillate fractions separated from the products may be atmospheric distillates only, but it is preferred to separate a vacuum distillate from the products as well.
  • the separated vacuum distillate may be converted into light hydrocarbon distillates in the manners described hereinbefore.
  • a heavy fraction from the cracked product from the cracking unit in which the relatively low asphaltenes feed is processed will preferably be recirculated to that cracking unit.
  • a relatively low-asphaltenes heavy fraction may, if desired, be separated from the product obtained in the cracking unit in which the relatively asphaltenes-rich feed is cracked and be used as a feed component for the cracking unit in which the relatively low-asphaltenes feed is processed.
  • the TC treatment both of relatively low-asphaltenes feeds and of relatively asphaltenes-rich feeds should preferably be carried out at a temperature of from 400-525°C and a space velocity of from 0.01-5 kg fresh feed per litre cracking reactor volume per minute.
  • class I may be subdivided depending on whether stream 2 is used as the feed for the DA treatment (class IA), or as a feed component for the TC treatment (class IB). In the embodiments falling within class IB stream 5 is used as the feed for the DA treatment.
  • FIG. 1 The various embodiments falling within class IA are illustrated schematically in Figure I.
  • the various streams, fractions and reaction zones are indicated by three digit numbers, the first of which refers to the Figure concerned.
  • the vacuum residue (302) for instance, refers to stream 2 as described hereinbefore in the context of Figure 3.
  • the process is carried out in an apparatus comprising a HT zone (106), a DA zone (107) and a TC zone (108), successively.
  • An asphaltenes-containing hydrocarbon mixture (101) is subjected to a HT and the hydrotreated product is separated into one or more distillate fractions (109) and a residual fraction (102).
  • Stream 102 is subjected to a DA treatment and the product is separated into a deasphalted oil (103) and an asphaltic bitumen (104).
  • Stream 103 is subjected to a TC treatment and the cracked product is separated into one or more distillate fractions (110) and a residual fraction (105).
  • Figure I includes the following seven embodiments:
  • FIG. II The various embodiments falling within class IB are represented schematically in Figure II. According to this Figure the process is carried out in an apparatus comprising a HT zone (206), a TC zone (207) and a DA zone (208).
  • An asphaltenes-containing hydrocarbon mixture (201) is subjected to a HT and the hydrotreated product is separated into one or more distillate fractions (209) and a residual fraction (202).
  • Stream 202 is subjected to a TC treatment and the cracked product is separated into one or more distillate fractions (210) and a residual fraction (205).
  • Stream 205 is subjected to a DA treatment and the product is separated into a deasphalted oil (203) and an asphaltic bitumen (204).
  • Stream 203 is used as a feed component for the TC treatment.
  • Stream 203 in addition to this embodiment (IB1), in which stream 204 is not subjected to further processing Figure II includes another embodiment (IB2) in which at least part of stream 204 is used as a feed component for the HT.
  • bleed stream should preferably be separated from one of the heavy streams of the process. In this way the build-up of undesirable heavy components during the process can be obviated.
  • the process is carried out in an apparatus comprising, successively a HT zone composed of a unit for catalytic hydrotreatment (306), a unit for atmospheric distillation (307) and a unit for vacuum distillation (308), a DA zone (309) and a TC zone composed of a thermal cracking unit (310), a second unit for atmospheric distillation (311) and a second unit for vacuum distillation (312).
  • An asphaltenes-containing hydrocarbon mixture (301) is mixed with a recirculation stream (313) and the mixture (314) is subjected together with hydrogen (315) to a catalytic hydrotreatment.
  • the hydrotreatment product (316) is separated by atmospheric distillation into a gas fraction (317), an atmospheric distillate (318) and an atmospheric residue (319).
  • the atmospheric residue (319) is separated by vacuum distillation into a vacuum distillate (320) and a vacuum residue (302).
  • the vacuum residue (302) is separated by solvent deasphalting into a deasphalted oil (303) and an asphaltic bitumen (304).
  • the deasphalted oil (303) is mixed with an atmospheric residue (321) and the mixture (322) is subjected to thermal cracking.
  • the asphaltic bitumen (304) is divided into two portions (323) and (324) and portion (324) is mixed with a vacuum residue (305) to form the recirculation stream (313).
  • the thermally cracked product (325) is separated by atmospheric distillation into a gas fraction (326), an atmospheric distillate (327) and an atmospheric residue (328).
  • the atmospheric residue (328) is divided into two portions (321) and (329) and portion (329) is separated by vacuum distillation into a vacuum distillate (330) and a vacuum residue (305).
  • the process is carried out in an apparatus comprising, successively, a HT zone composed of a unit for catalytic hydrotreatment (406), a unit for atmospheric distillation (407) and a unit for vacuum distillation (408), a DA zone (409) and a TC zone composed of a thermal cracking unit (410), a second unit for atmospheric distillation (411), a second thermal cracking unit (412), a third unit for atmospheric distillation (413) and a second unit for vacuum distillation (414).
  • An asphaltenes-containing hydrocarbon mixture (401) is mixed with a vacuum residue (415) and the mixture (416) is subjected together with hydrogen (417) to a catalytic hydrotreatment.
  • the hydrotreated product (418) is separated by atmospheric distillation into a gas fraction (419), an atmospheric distillate (420) and an atmospheric residue (421).
  • the atmospheric residue (421) is separated by vacuum distillation into a vacuum distillate (422) and a vacuum residue (402).
  • the vacuum residue (402) is separated by solvent deasphalting into a deasphalted oil (403) and an asphaltic bitumen (404).
  • the deasphalted oil (403) is mixed with atmospheric residue (423) and the mixture (424) is converted in the second thermal cracking unit into a product (425) which is split up by atmospheric distillation into a gas fraction (426), an atmospheric distillate (427) and an atmospheric residue (428).
  • the atmospheric residue (428) is divided into two portions (423) and (429).
  • the asphaltic bitumen (404) is converted in the first thermal cracking unit into a product (430) which is separated by atmospheric distillation into a gas fraction (431) an atmospheric distillate (432) and an atmospheric residue (433). Gas fractions (426) and (431) are combined to form mixture (434).
  • Atmospheric distillates (427) and (432) are combined to form mixture (435). Atmospheric residues (429) and (433) are combined to form mixture (436) which is separated by vacuum distillation into a vacuum distillate (437) and a vacuum residue (405). Vacuum residue (405) is divided into two portions (415) and (438).
  • the process is carried out in an apparatus comprising, successively, a HT zone composed of a unit for catalytic hydrotreatment (506), an atmospheric distillation unit (507) and a vacuum distillation unit (508), a TC zone composed of a thermal cracking unit (509), a second atmospheric distillation unit (510), a second thermal cracking unit (511), a third atmospheric distillation unit (512) and a second vacuum distillation unit (513), and a DA zone (514).
  • An asphaltenes-containing hydrocarbon mixture (501) is mixed with an asphaltic bitumen (515) and the mixture (516) is subjected, together with hydrogen (517) to a catalytic hydrotreatment.
  • the hydrotreated product (518) is separated by atmospheric distillation into a gas fraction (519), an atmospheric distillate (520) and an atmospheric residue (521).
  • the atmospheric residue (521) is separated by vacuum distillation into a vacuum distillate (522) and a vacuum residue (502).
  • the vacuum residue (502) is converted by thermal cracking into a product (523) which by atmospheric distillation is separated into a gas fraction (524), an atmospheric distillate (525) and an atmospheric residue (526).
  • the atmospheric residue (526) is mixed with an atmospheric residue (527) and the mixture (528) is separated by vacuum distillation into a vacuum distillate (529) and a vacuum residue (505).
  • the vacuum residue (505) is separated by solvent deasphalting into a deasphalted oil (503) and an asphaltic bitumen (504).
  • the deasphalted oil (503) is mixed with an atmospheric residue (530) and the mixture (531) is subjected to thermal cracking to form a product (532) which by atmospheric distillation is separated into a gas fraction (533), an atmospheric distillate (534) and an atmospheric residue (535).
  • the atmospheric residue (535) is divided into two portions (527) and (530).
  • Gas fractions (524) and (533) are combined to form mixture (536).
  • Atmospheric distillates (525) and (534) are combined to form mixture (537).
  • Asphaltic bitumen (504) is divided into two portions (515) and (538).
  • the present patent application also includes apparatuses for carrying out the process according to the invention substantially corresponding with those schematically represented in Figures I-V.
  • the starting mixtures used in the process according to the invention were three asphaltenes-containing hydrocarbon mixtures obtained as residues in the vacuum distillation of atmospheric distillation residues from crude mineral oils from the Middle East. All three vacuum residues boiled substantially above 520°C; they had RCT's of 18.8,14.5 and 17.1 % w, respectively.
  • the process was carried out according to flow diagrams A-C. The following conditions were used in the various zones:
  • the TC treatment was carried out in one or two cracking coils at a pressure of 20 bar and a space velocity of 0.4 kg fresh feed per litre cracking coil volume per minute.

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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)
EP82201560A 1981-12-10 1982-12-07 Process for the production of hydrocarbon oil distillates Expired EP0082551B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
NL8105560 1981-12-10
NL8105560A NL8105560A (nl) 1981-12-10 1981-12-10 Werkwijze voor de bereiding van koolwaterstofoliedestillaten.

Publications (2)

Publication Number Publication Date
EP0082551A1 EP0082551A1 (en) 1983-06-29
EP0082551B1 true EP0082551B1 (en) 1986-02-19

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EP82201560A Expired EP0082551B1 (en) 1981-12-10 1982-12-07 Process for the production of hydrocarbon oil distillates

Country Status (11)

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EP (1) EP0082551B1 (es)
JP (1) JPS58108295A (es)
AR (1) AR247915A1 (es)
AU (1) AU553542B2 (es)
CA (1) CA1198388A (es)
DE (1) DE3269261D1 (es)
ES (1) ES8308585A1 (es)
MX (1) MX162957B (es)
NL (1) NL8105560A (es)
SU (1) SU1306479A3 (es)
ZA (1) ZA829036B (es)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL8201233A (nl) * 1982-03-24 1983-10-17 Shell Int Research Werkwijze voor de bereiding van asfaltenenarme koolwaterstofmengsel.
CA2117571A1 (en) * 1993-08-30 1995-03-01 Junichi Kubo Process for hydrotreating heavy hydrocarbon oil
FR2906812A1 (fr) * 2006-10-06 2008-04-11 Inst Francais Du Petrole Procede de conversion de residu desasphalte par craquage thermique
US20140221713A1 (en) * 2013-02-04 2014-08-07 Lummus Technology Inc. Residue hydrocracking processing

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3549517A (en) * 1968-07-23 1970-12-22 Hydrocarbon Research Inc High conversion level hydrogenation of residuum
US3730875A (en) * 1971-02-16 1973-05-01 Universal Oil Prod Co Combination process for black oil conversion
US3723297A (en) * 1971-10-18 1973-03-27 Universal Oil Prod Co Conversion of asphaltene-containing charge stocks
NL7612960A (nl) * 1976-11-22 1978-05-24 Shell Int Research Werkwijze voor het omzetten van koolwater- stoffen.
JPS541306A (en) * 1977-06-07 1979-01-08 Chiyoda Chem Eng & Constr Co Ltd Hydrogenation of heavy hydrocarbon oil
GB2031011B (en) * 1978-10-05 1983-01-06 Chiyoda Chem Eng Construct Co Processing heavy hydrocarbon oils

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Publication number Publication date
NL8105560A (nl) 1983-07-01
EP0082551A1 (en) 1983-06-29
DE3269261D1 (en) 1986-03-27
ZA829036B (en) 1984-05-30
ES517987A0 (es) 1983-09-01
CA1198388A (en) 1985-12-24
JPS58108295A (ja) 1983-06-28
ES8308585A1 (es) 1983-09-01
AU9133382A (en) 1983-06-16
AR247915A1 (es) 1995-04-28
AU553542B2 (en) 1986-07-17
MX162957B (es) 1991-07-22
JPH0581636B2 (es) 1993-11-15
SU1306479A3 (ru) 1987-04-23

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