US3775294A - Producing coke from hydrotreated crude oil - Google Patents

Producing coke from hydrotreated crude oil Download PDF

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Publication number
US3775294A
US3775294A US00157529A US3775294DA US3775294A US 3775294 A US3775294 A US 3775294A US 00157529 A US00157529 A US 00157529A US 3775294D A US3775294D A US 3775294DA US 3775294 A US3775294 A US 3775294A
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crude oil
crude
hydrotreating
oil
coker
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US00157529A
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A Peterson
F Dormish
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Marathon Oil Co
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Marathon Oil Co
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
    • C10B57/04—Other carbonising or coking processes; Features of destructive distillation processes in general using charges of special composition
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B55/00—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material

Definitions

  • the present invention relates generally to the field of hydrocarbon conversion processes and more specifically to hydrotreating and coking generally classified in the United States Patent Oflice, Class 208 subclass 212.
  • Netherlands patent NL-6916 218-Q which claims priority of U.S. patent application 771,248, filed Oct. 28, 1968, teaches processes for converting sulfurous, hydrocarbonaceous black oils into lower boiling, normally liquid-hydrocarbon products of reduced sulfur content with an integrated process involving cracking in the presence of hydrogen and fixed bed catalytic desulfurization.
  • Netherlands patent NL-6916 017-Q which claims priority of U.S. patent application Ser. No. 770,724, filed Oct. 25, 1968, teaches hydrodesulfurization of crude oil or reduced crude containing asphaltene fractions at low temperatures in the presence of a Group VI/ Group VII metal catalyst on alumina.
  • the advantages of the invention include: capital cost saving by reducing number of fractionating columns and number of hydrotreating units required; reduced quantities of coke and corresponding increases in quantities of more valuable liquid products; lower sulfur content in the coke, in the C and lighter overheads and in all other liquid products; reduced corrosion due to sulfur removal before contact with crude tower, coker and subsequent downstream processing units; high throughput through the hydrotreater (the light fractions are hydrotreated in a unit no larger than that required for conventional hydrotreating of the heavier fractions only); and lower olefin contents in naphtha products, particularly gasoline.
  • the present invention provides coke, particularly low sulfur coke which is of special value in the production of electrodes, e.g., for the electrolytic production of aluminum, and also produces low-sulfur liquid products which can be refined into naphthas, particularly gasoline having lower olefin contents.
  • FIG. 1 is a schematic drawing of a refinery system hydrotreating whole crude oil of the present invention.
  • FIG. 2 shows a schematic diagram of a process for hydrotreating topped crude oil according to the invention.
  • Hydrocarbons It is an important aspect of the present invention that whole crude oil is hydrotreated. Previous processes have hydrotreated residual, e.g., 650 F. plus portions without achieving the advantages of the present invention as is demonstrated by a comparison of Examples HI and V. Crudes which are partially useful for the practice of the invention are those which are relatively high in sulfur content but low in asphaltene and heavy metals content. Sour West Texas crude is a good example of this type of crude.
  • Topped crudes e.g., those having the portion boiling below about 400 F. fractioned out, can be utilized in place of the whole crude oil.
  • Residual fraction the preferred residual fraction for coking according to the present invention is the fraction generally boiling above about 900 F., more preferably above about 1000 F., and most preferably above about 1050 F.
  • Coker liquid products the coker liquid products selected for recycle will generally consist of the entire liquid product from C or C up through the highest boiling liquid products produced.
  • the lower molecular weight material, particularly the C C and perhaps C portion are advantageously separated for olefin recovery. Any other portions of the coker liquid product may also be separated for separate use, if desired. From about 1 to about 100, more preferably from 50 to about 100, and most preferably from 75 to about 100 volume percent of liquid (C -plus) products from the coker will be mixed with the whole crude entering the hydrotreating process.
  • the remaining coker liquids, if any, can be utilized for conventional purposes, e.g., for gasoline and heavier fuels.
  • the hydrogen utilized with the present invention can be of commercial purity such as that derived from the reforming of naphtha as by any of the reforming processes described on pp. 184-193 of the September 1970 issue of Hydrocarbon Processing or can be manufactured specially for the purpose such as by steam reforming or partial oxidation of hydrocarbons (ibid. pp. 269-270). From about 1000 to about 6000, more preferably about 2000 to about 5000, and most preferably from about 2500 to about 4000 standard cubic feet of hydrogen will be contacted with each barrel of crude oil.
  • Catalyst A wide variety of hydrogenation catalysts, especially those containing metals selected from the group nickel, molybdenum, cobalt and tungsten, or compounds containing such metals, can be employed including those marketed by the Girdler Division of Chemetron Corp. under the trade name Girdler G-51, Girdler G-76; those marketed by Union Oil Company of California under the trade name N-12; those marketed by American Cyanamid Company under the trade name Cyanamid HDS-ZA and Cyanamid EDS-1450, Cyanamid HTS- 1441, Cyanamid HDS-9A, and Cyanamid HDS-BA; those marketed by the Davison Chemical Company, Division of W. R. Grace & Co.
  • nickel-molybdenum catalysts e.g., American Cyanamid HDS-3, EDS-9A and Nalco NM-502 are most preferred.
  • Catalyst support The preferred catalyst supports are alumina, silica, magnesia or combinations thereof. In general, the support should not be sufficiently acidic so as to cause extensive hydrocracking of the oil under the preferred reaction conditions.
  • a catalyst in the form of an extrudate, pellet or sphere of such size as to avoid excessive pressure drop through the catalyst bed but small enough to provide good transport of the oil into the center of the catalyst particle is used. Sizes from about /s to 1 inch are generally preferred. In a moving or ebulating bed hydrotreating reactor, inch or smaller extrudates or other shaped particles can be used to advantage.
  • the temperature during the hydrotreating reaction should be from 600 to about 850 F., more preferably from 650 to about 800 F., and most preferably from 675 to about 775 F.
  • the temperature used will depend on the relative hydrodesulfurization and hydrocracking activities of the particular catalyst used and will normally be increased during a run to compensate for catalyst deactivation.
  • pressure during the hydrotreating reaction should be from about 250 to about 5000, more preferably from about 600 to about 2500 and most preferably from 800 to about 2000 p.s.1.g.
  • Liquid hourly space velocity will generally be in the range of from about 4 0.5 to about 6, more preferably 0.5 to about 4, and most preferably 1 to about 3 volumes of liquid per volume of hydrotreating catalyst per hour.
  • Coking The coking is carried out under conventional conditions, e.g., those described on pages -181 of the September 1970 issue of Hydrocarbon Processing and in the references therein.
  • Conventional hydrotreating, distillation and coking apparatus can be employed. Though not necessary to the invention, with crude having high content of metals and/ or particulates, a conventional guard case filled with inexpensive catalyst can be provided upstream of the main hydrotreating reactor to protect the more expensive main catalyst.
  • Examples I, IV and V are according to the invention.
  • Examples II and III are comparative examples to illustrate the loss of advantages when the crude oil is first fractionated and the fractions separately hydrotreated.
  • EXAMPLE I (Hydrotreating whole crude according to the invention) Referring to FIG. 1, whole crude 10 enters the desalter 11 of conventional design which removes inorganic halides.
  • the desalted crude is heatcd in heat exchanger 12, contacted with make-up hydrogen 14 and recycle hydrogen 33 and further heated in furnace 13.
  • the hot crude plus hydrogen stream is passed over a bed of nickel-molybdenum catalyst in hydrotreater 15 where hydrotreating occurs.
  • the hydrotreated stream is cooled in heat exchanger 16 and fed to separator 17 which separates the gaseous from the liquid products.
  • the liquid products are fed to the main distillation columns 18 where they are fractionated into product streams; gas 19 (composed primarily of C through 0.; which is sent to a conventional gas concentration facility), gasoline 20 (composed primarily of C through C fractions boiling up to about 400 F. and which is sent to blending and/or catalytic reforming).
  • middle distillate 21 (which may be more than one fraction and which is composed primarily of kerosene, diesel fuel, and jet fuel)
  • gas oil 22 both atmospheric and vacuum gas oil which is sent to catalytic cracking or to hydrocracking and residuals 23 which are sent to conventional delayed coker 24 to produce coke 25).
  • Overhead from the coker is sent to heat exchanger 26 where it is cooled before fractionation in fractionating column 27.
  • Overhead 28 from column 27 is composed primarily of C and lighter hydrocarbons and is sent to gas concentration.
  • the bottoms 29 from fractionating tower 27 are composed primarily of C and heavier hydrocarbons and are recycled back to mix with the efiluent from desalter 11.
  • the gaseous efiluent 30 from separator 17 is sent to scrubber 31 which removes a stream 32 consisting primarily of hydrogen sulfide and ammonia.
  • the remainder of the efiluent from scrubber 31 consists primarily of hydrogen 33 which is recycled to mix with the make-up hydrogen and liquid feed to the hydrotreater 15.
  • a crude oil containing 1.67 weight percent sulfur is processed according to this invention as shown in FIG. 1, to yield low sulfur liquid products and a delayed coke of reduced sulfur content.
  • the sulfur contents of various fractions of the raw crude oil are shown in the table below.
  • the hydrotreater 15 is operatedat 700 C. and 1500 p.s.i.g. with a total hydrogen feed of 3350 standard cubic feet per barrel of. oil.
  • the oil is fed at a liquid hourly space velocity of 1.7 hr.”
  • the catalyst used is American Cyanamid HDS-3A.
  • the feed to thecoking unit 24 consists of residual boiling-iabove about 975 F. from column 18.
  • the delayed coking unit 24 is Operated at a 925 F. bed temperature .and inlet feed temperature of 1000 F.
  • the oil to steam feedratio is 20.5 volume of oil to volume of water. Cokingtime is 9 hours.
  • the total charge to the hydrotreating unit 15 is 1185 bbl. per day.
  • the additional charge rate of 185 bbl. per day is the recycled coker condensate 29.
  • EXAMPLE II V (Conventionally fractionating and coking without hydrotreating) The same crude oil used in Example I is conventionally distilled and the residual fraction is coked under the conditions of Example I. Yields and sulfur contents of the products are tabulated below.
  • the portion of the crude oil of Example I boiling above 400 F. is hydrotreated over the catalyst of Example III under substantially identical conditions except that the liquid hourly space velocity of the total feed is increased such that the space velocity of just the 630 F. plus portion of the feed is substantially the same as in Example 111.
  • the lower sulfur contents of the 600-l050 F. and residual (1050 F. plus) fractions of the product of Example IV show the advantage of processing the. 400-600 F. portion of the crude oil together with the atmospheric residual (630 F. plus) fraction. No increase in hydrotreating reactor size is required since the space velocity can be increased sufficiently to include this additional material and still obtain improved desulfurization of the residual. Only a small amount of product boiling below 400 F. is obtained.
  • EXAMPLE V (Demonstrating the advantages of hydrotreating whole crude oil as opposed to atmospheric residual)
  • the whole crude oil of Example I is hydrotreated under essentially identical conditions as in Example IH, except that the liquid hourly space velocity of the total feed is increased sufficiently that more of the 630 F. plus portion of the crude oil is being hydrotreated per day than in Example III using the same size reactor.
  • the sulfur content of all of the product fractions is equal to or lower than the corresponding products of Example HI despite the processing of both the lighter portion of the crude and a somewhat greater amount per day of 630 F. plus atmospheric residual.
  • said hydrotreating catalyst comprises a metal selected from the group consisting of nickel, molybdenum, cobalt and tungsten or a compound containing one of the foregoing metals.
  • feed to said hydrotreater consists essentially of topped crude oil, recycle bottoms from said fractionation of said coker oT erheads, and hydrogen.
  • step (a) can consist essentially of whole c rude oil.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
US00157529A 1971-06-28 1971-06-28 Producing coke from hydrotreated crude oil Expired - Lifetime US3775294A (en)

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Cited By (31)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3984305A (en) * 1973-04-12 1976-10-05 Kureha Kagaku Kogyo Kabushiki Kaisha Process for producing low sulfur content fuel oils
US4048053A (en) * 1975-10-30 1977-09-13 Cities Service Company Upgrading solid fuel-derived tars produced by short residence time low pressure hydropyrolysis
US4358361A (en) * 1979-10-09 1982-11-09 Mobil Oil Corporation Demetalation and desulfurization of oil
US4388175A (en) * 1981-12-14 1983-06-14 Texaco Inc. Hydrocarbon conversion process
US4388152A (en) * 1980-08-04 1983-06-14 Conoco Inc. Process for producing blast furnace grade coke, a distillable product and fuel gases from a heavy, high sulfur, crude oil
US4455221A (en) * 1983-02-09 1984-06-19 Intevep Process for upgrading heavy hydrocarbons employing a diluent
US4498974A (en) * 1982-09-17 1985-02-12 Institut Francais Du Petrole Process for converting a highly viscous hydrocarbon charge to a less viscous, more easily transportable and more easily refinable hydrocarbon fraction
DE3725764A1 (de) * 1986-08-04 1988-02-25 Intevep Sa Verfahren und anlage zum erzeugen von koks in anodenqualitaet
US6168709B1 (en) 1998-08-20 2001-01-02 Roger G. Etter Production and use of a premium fuel grade petroleum coke
US20060032788A1 (en) * 1999-08-20 2006-02-16 Etter Roger G Production and use of a premium fuel grade petroleum coke
US20090145810A1 (en) * 2006-11-17 2009-06-11 Etter Roger G Addition of a Reactor Process to a Coking Process
US20090152165A1 (en) * 2006-11-17 2009-06-18 Etter Roger G System and Method for Introducing an Additive into a Coking Process to Improve Quality and Yields of Coker Products
US20090209799A1 (en) * 2006-11-17 2009-08-20 Etter Roger G System and Method of Introducing an Additive with a Unique Catalyst to a Coking Process
US20100170827A1 (en) * 2006-11-17 2010-07-08 Etter Roger G Selective Cracking and Coking of Undesirable Components in Coker Recycle and Gas Oils
US9011672B2 (en) 2006-11-17 2015-04-21 Roger G. Etter System and method of introducing an additive with a unique catalyst to a coking process
US20180016503A1 (en) * 2016-07-15 2018-01-18 Indian Oil Corporation Limited Delayed coker drum and method of operating thereof
US10808184B1 (en) 2016-11-03 2020-10-20 Marathon Petroleum Company Lp Catalytic stripping process
US11802257B2 (en) 2022-01-31 2023-10-31 Marathon Petroleum Company Lp Systems and methods for reducing rendered fats pour point
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US11891581B2 (en) 2017-09-29 2024-02-06 Marathon Petroleum Company Lp Tower bottoms coke catching device
US11898109B2 (en) 2021-02-25 2024-02-13 Marathon Petroleum Company Lp Assemblies and methods for enhancing control of hydrotreating and fluid catalytic cracking (FCC) processes using spectroscopic analyzers
US11905479B2 (en) 2020-02-19 2024-02-20 Marathon Petroleum Company Lp Low sulfur fuel oil blends for stability enhancement and associated methods
US11905468B2 (en) 2021-02-25 2024-02-20 Marathon Petroleum Company Lp Assemblies and methods for enhancing control of fluid catalytic cracking (FCC) processes using spectroscopic analyzers
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Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4178229A (en) * 1978-05-22 1979-12-11 Conoco, Inc. Process for producing premium coke from vacuum residuum

Cited By (51)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3984305A (en) * 1973-04-12 1976-10-05 Kureha Kagaku Kogyo Kabushiki Kaisha Process for producing low sulfur content fuel oils
US4048053A (en) * 1975-10-30 1977-09-13 Cities Service Company Upgrading solid fuel-derived tars produced by short residence time low pressure hydropyrolysis
US4358361A (en) * 1979-10-09 1982-11-09 Mobil Oil Corporation Demetalation and desulfurization of oil
US4388152A (en) * 1980-08-04 1983-06-14 Conoco Inc. Process for producing blast furnace grade coke, a distillable product and fuel gases from a heavy, high sulfur, crude oil
US4388175A (en) * 1981-12-14 1983-06-14 Texaco Inc. Hydrocarbon conversion process
US4498974A (en) * 1982-09-17 1985-02-12 Institut Francais Du Petrole Process for converting a highly viscous hydrocarbon charge to a less viscous, more easily transportable and more easily refinable hydrocarbon fraction
US4455221A (en) * 1983-02-09 1984-06-19 Intevep Process for upgrading heavy hydrocarbons employing a diluent
DE3725764A1 (de) * 1986-08-04 1988-02-25 Intevep Sa Verfahren und anlage zum erzeugen von koks in anodenqualitaet
US6168709B1 (en) 1998-08-20 2001-01-02 Roger G. Etter Production and use of a premium fuel grade petroleum coke
US20060032788A1 (en) * 1999-08-20 2006-02-16 Etter Roger G Production and use of a premium fuel grade petroleum coke
US9475992B2 (en) 1999-08-20 2016-10-25 Roger G. Etter Production and use of a premium fuel grade petroleum coke
US9187701B2 (en) 2006-11-17 2015-11-17 Roger G. Etter Reactions with undesirable components in a coking process
US20090145810A1 (en) * 2006-11-17 2009-06-11 Etter Roger G Addition of a Reactor Process to a Coking Process
US20100170827A1 (en) * 2006-11-17 2010-07-08 Etter Roger G Selective Cracking and Coking of Undesirable Components in Coker Recycle and Gas Oils
US8206574B2 (en) 2006-11-17 2012-06-26 Etter Roger G Addition of a reactor process to a coking process
US8361310B2 (en) 2006-11-17 2013-01-29 Etter Roger G System and method of introducing an additive with a unique catalyst to a coking process
US8372265B2 (en) 2006-11-17 2013-02-12 Roger G. Etter Catalytic cracking of undesirable components in a coking process
US8372264B2 (en) 2006-11-17 2013-02-12 Roger G. Etter System and method for introducing an additive into a coking process to improve quality and yields of coker products
US8394257B2 (en) 2006-11-17 2013-03-12 Roger G. Etter Addition of a reactor process to a coking process
US8888991B2 (en) 2006-11-17 2014-11-18 Roger G. Etter System and method for introducing an additive into a coking process to improve quality and yields of coker products
US8968553B2 (en) 2006-11-17 2015-03-03 Roger G. Etter Catalytic cracking of undesirable components in a coking process
US9011672B2 (en) 2006-11-17 2015-04-21 Roger G. Etter System and method of introducing an additive with a unique catalyst to a coking process
US9150796B2 (en) 2006-11-17 2015-10-06 Roger G. Etter Addition of a modified vapor line reactor process to a coking process
US20090152165A1 (en) * 2006-11-17 2009-06-18 Etter Roger G System and Method for Introducing an Additive into a Coking Process to Improve Quality and Yields of Coker Products
US20090209799A1 (en) * 2006-11-17 2009-08-20 Etter Roger G System and Method of Introducing an Additive with a Unique Catalyst to a Coking Process
US20180016503A1 (en) * 2016-07-15 2018-01-18 Indian Oil Corporation Limited Delayed coker drum and method of operating thereof
US10501692B2 (en) * 2016-07-15 2019-12-10 Indian Oil Corporation Limited Delayed coker drum and method of operating thereof
US10808184B1 (en) 2016-11-03 2020-10-20 Marathon Petroleum Company Lp Catalytic stripping process
US11168270B1 (en) 2016-11-03 2021-11-09 Marathon Petroleum Company Lp Catalytic stripping process
US11891581B2 (en) 2017-09-29 2024-02-06 Marathon Petroleum Company Lp Tower bottoms coke catching device
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US11920096B2 (en) 2020-02-19 2024-03-05 Marathon Petroleum Company Lp Low sulfur fuel oil blends for paraffinic resid stability and associated methods
US11905479B2 (en) 2020-02-19 2024-02-20 Marathon Petroleum Company Lp Low sulfur fuel oil blends for stability enhancement and associated methods
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US12031094B2 (en) 2021-02-25 2024-07-09 Marathon Petroleum Company Lp Assemblies and methods for enhancing fluid catalytic cracking (FCC) processes during the FCC process using spectroscopic analyzers
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US12163878B2 (en) 2021-02-25 2024-12-10 Marathon Petroleum Company Lp Methods and assemblies for determining and using standardized spectral responses for calibration of spectroscopic analyzers
US11970664B2 (en) 2021-10-10 2024-04-30 Marathon Petroleum Company Lp Methods and systems for enhancing processing of hydrocarbons in a fluid catalytic cracking unit using a renewable additive
US12338396B2 (en) 2021-10-10 2025-06-24 Marathon Petroleum Company Lp Methods and systems for enhancing processing of hydrocarbons in a fluid catalytic cracking unit using a renewable additive
US12297403B2 (en) 2022-01-31 2025-05-13 Marathon Petroleum Company Lp Systems and methods for reducing rendered fats pour point
US11802257B2 (en) 2022-01-31 2023-10-31 Marathon Petroleum Company Lp Systems and methods for reducing rendered fats pour point
US12311305B2 (en) 2022-12-08 2025-05-27 Marathon Petroleum Company Lp Removable flue gas strainer and associated methods
US12306076B2 (en) 2023-05-12 2025-05-20 Marathon Petroleum Company Lp Systems, apparatuses, and methods for sample cylinder inspection, pressurization, and sample disposal

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DE2215664B2 (de) 1974-10-31
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