WO2000063320A1 - Procede ameliore de desasphaltage de residus faisant appel a un recyclage reactif d'une matiere a point d'ebullition eleve - Google Patents

Procede ameliore de desasphaltage de residus faisant appel a un recyclage reactif d'une matiere a point d'ebullition eleve Download PDF

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Publication number
WO2000063320A1
WO2000063320A1 PCT/US2000/009607 US0009607W WO0063320A1 WO 2000063320 A1 WO2000063320 A1 WO 2000063320A1 US 0009607 W US0009607 W US 0009607W WO 0063320 A1 WO0063320 A1 WO 0063320A1
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WO
WIPO (PCT)
Prior art keywords
solids
residence time
reaction zone
zone
fraction
Prior art date
Application number
PCT/US2000/009607
Other languages
English (en)
Inventor
Mitchell Jacobson
Willibald Serrand
Norman Harris Sweed
Hans Weiss
Ingo Dreher
Udo Zentner
Jorg Schmalfeld
Original Assignee
Exxonmobil Research And Engineering Company
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Exxonmobil Research And Engineering Company filed Critical Exxonmobil Research And Engineering Company
Priority to EP00925922.7A priority Critical patent/EP1194498B1/fr
Priority to AU44542/00A priority patent/AU771590B2/en
Priority to ES00925922.7T priority patent/ES2559272T3/es
Priority to CA2370591A priority patent/CA2370591C/fr
Priority to JP2000612401A priority patent/JP4590108B2/ja
Publication of WO2000063320A1 publication Critical patent/WO2000063320A1/fr

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Classifications

    • 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
    • C10G9/00—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
    • C10G9/28—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid material
    • C10G9/32—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid material according to the "fluidised-bed" technique
    • 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

Definitions

  • the present invention relates to an improved process for deasphalting a residua feedstock by use of a short vapor residence time process unit comprised of a horizontal moving bed of fluidized and/or stirred hot particles.
  • the vapor phase product stream from said process unit is passed to a soaker drum where a high boiling fraction is separated and recycled to the process unit after undergoing reactions causing molecular weight growth.
  • This reactive recycle using the soaker drum results in substantially improved qualities of the liquid products compared with what is achieved by once-through residua deasphalting process alternatives.
  • crude oils are subjected to atmospheric distillation to separate lighter materials such as gas oils, kerosenes, gasolines, straight run naphtha, etc. from the heavier materials.
  • the residue from the atmospheric distillation step is then distilled at a pressure below atmospheric pressure.
  • This later distillation step produces a vacuum gas oil distillate and a vacuum reduced residual oil which often contains relatively high levels of asphaltene molecules.
  • asphaltene molecules usually contain most of the Conradson Carbon residue and metal components of the resid. They also contain relatively high levels of heteroatoms, such as sulfur and nitrogen.
  • Such feeds have little commercial value, primarily because they cannot be used as a fuel oil because of ever stricter environmental regulations.
  • U.S. Patent No. 4,191,639 to Audeh et al teaches a process wherein hydrocarbon oils, such as residual petroleum oils, are deasphalted and demetallized by contact with a liquid mixture of at least two of the components selected from hydrogen sulfide, carbon dioxide, and propane.
  • US Patent 5,714,056 teaches a process for deasphalting residua in a short vapor contact time thermal process unit comprised of a horizontal moving bed of fluidized hot particles. This is a once through process whereby the removal of feed contaminants is limited to what can be achieved in a single pass. There is no suggestion of separating a high boiling fraction from the vapor product fraction and recycling it to the reaction zone.
  • a process for deasphalting an asphalt-containing feedstock in a deasphalting process unit comprised of: (i) a heating zone wherein solids containing carbonaceous deposits are received from a stripping zone and heated in the presence of a heating gas which may contain oxygen for partial combustion purposes;
  • a short vapor residence time reaction zone containing a horizontal moving bed of fluidized and/or stirred hot solids recycled from the heating zone and feed, which reaction zone is operated at a temperature from about 450°C to about 700°C and operated under conditions such that the solids residence time and the vapor residence time are independently controlled, which vapor residence time is less than about 5 seconds, and which solids residence is from about 5 to about 60 seconds;
  • step (f) passing the vaporized fraction from step (b) above to a soaker drum where it is quenched to produce a vapor fraction boiling less than about 450-600°C and a high boiling fraction condensate having an initial boiling point in the range of about 450-600°C;
  • step (i) recovering the vapor fraction having a lower concentration of contaminants from step (h).
  • steam, C4 minus gas, or both is injected into the soaker drum to maintain the solids in suspension and to strip out lower boiling range products.
  • the soaker drum is operated at increased pressure and temperature to reduce reaction time and therefore the soaker drum size.
  • the particles of the short contact time reaction zone are fluidized and/or stirred with the aid of a mechanical means.
  • steam, C minus gas, or both are injected into the vaporized fraction upstream of the soaker drum to reduce the partial pressure of the C 5 plus hydrocarbon to -condense the high boiling fraction as per step (f) at a temperature which is lower than its initial boiling point of about 450-600°C.
  • polymerization initiators are present in the soaker drum to increase reaction rates.
  • the soaker drum can include a mechanical mixing device providing the advantages of self-cleaning to minimize coke deposits and to achieve substantially plug flow reaction conditions of the liquid phase.
  • Residua feedstocks which are upgraded in accordance with the present invention are those petroleum fractions boiling above about 380°C, preferably above about 540°C, more preferably above about 560°C.
  • Non- limiting examples of such fractions include vacuum resids, atmospheric resids, heavy and reduced petroleum crude oil; pitch; waste oils; asphalt; bitumen; solvent deasphalter residue; and tar sand oil. It is understood that such resids may also contain minor amounts of lower boiling material.
  • These feedstocks cannot be fed in substantial quantities to refinery process units, such as FCC units, because they are typically high in Conradson Carbon and they usually contain an undesirable amount of metal-containing components.
  • Conradson Carbon residues will deposit on the FCC cracking catalyst and cause excessive deactivation. Metals, such as nickel and vanadium will also deactivate the catalyst by acting as catalyst poisons. Such feeds will typically have a Conradson Carbon content of at least 5 wt.%, generally from about 5 to 50 wt.%. As to Conradson Carbon residue, see ASTM Test D 189- 165.
  • Residuum feedstocks are upgraded in accordance with the present invention in a short vapor residence time process unit which is comprised of a heating zone, a short vapor residence time horizontal fluidized and/or stirred bed reaction zone and a stripping zone.
  • a short vapor residence time process unit which is comprised of a heating zone, a short vapor residence time horizontal fluidized and/or stirred bed reaction zone and a stripping zone.
  • a residual feedstock which is high in Conradson Carbon and/or metal-components is fed via line 10 to one or more short vapor residence time reaction zone 1 which contains a horizontal moving bed of fluidized and/or stirred hot solids. It is preferred that the solids in the short vapor residence time reactor are fluidized and/or stirred with assistance of mechanical means.
  • the reactor may be stripped by use of a stripping gas, such as steam, or C minus gas, or by the vapors resulting from the vaporization of a fraction of the feedstock.
  • a stripping gas such as steam, or C minus gas
  • the mechanical means be a self cleaning mechanical mixing system characterized as having a relatively high radial mixing efficiency with only minor amounts of axial backmixing. Such a mixing system acts like a plug flow system with a flow pattern which ensures that the residence time is nearly equal for all particles.
  • the most preferred mechanical mixer is the mixer referred to by Lurgi AG of Germany as the LR-Mixer or LR-Flash Coker which was originally designed for processing oil shale, coal, and tar sands.
  • the LR- Mixer consists of two or more horizontally oriented rotating screws which mix the feed and hot solids while stirring and transporting the mixture through the reactor.
  • the solid particles be coke particles, they may be any other suitable refractory particulate material.
  • suitable refractory materials include those selected from the group consisting of silica, alumina, zirconia, magnesia, mullite, synthetically prepared or naturally occurring material such as pumice, clay, kieselguhr, diatomaceous earth, bauxite, and the like.
  • the solids be inert or have catalytic properties.
  • the solids will preferably have an average particle size of about 40 microns to 2,000 microns, more preferably from about 200 microns to about 1000 microns.
  • the feedstock is contacted with the hot solids at a temperature from about 450°C to about 700°C, preferably from about 500°C to 600°C, more preferably from about 520°C to 600°C.
  • a substantial portion of the high Conradson Carbon and metal-containing components will deposit on the hot solid particles in the form of high molecular weight carbon and metal moieties.
  • the remaining portion will be vaporized on contact with the hot solids.
  • the residence time of vapor products in reaction zone 1 will be an effective amount of time so that substantial secondary cracking does not occur. This amount of time will typically be less than about 5 seconds, preferably less than about 2 seconds.
  • the residence time of solids in the reaction zone will be from about 5 to 60 seconds, preferably from about 10 to 30 seconds.
  • One novel aspect of the present invention is that the residence time of the solids and the residence time of the vapor products, in the reaction zone, are independently controlled. Most fluidized bed processes are designed so that the solids residence time, and the vapor residence time cannot be independently controlled, especially at relatively short vapor residence times. It is preferred that the short vapor residence time process unit be operated so that the ratio of solids to feed be from about 30 to 1 to 3 to 1, preferably about 5 to 1. It is to be understood that the precise ratio of solids to feed will primarily depend on the heat balance requirement of the short vapor residence time reaction zone and the temperature of the solids. Associating the oil to solids ratio with heat balance requirements is within the skill of those having ordinary skill in the art, and thus will not be elaborated herein any further.
  • the vaporized fraction is passed via line 11 to soaker drum 2 which is maintained at effective conditions so that the highest boiling materials are condensed out. Typically these conditions will include controlled quenching of the vapor fraction just below the dewpoint.
  • the condensate is maintained in the soaker drum for an effective amount of time and reaction severity to initiate polymerization to coke precursors.
  • a quench stream can also be passed into soaker drum via line 21.
  • the quench stream will typically be an oil stream ranging from naphtha (Cs/150 o C) to residuum stream (550°C+).
  • Preferred quench streams are fractionator bottoms having a boiling range of 300°C to 700°C.
  • Coke or polymerization initiators which include those selected from the group consisting of elemental sulfur, peroxides, and spent cracking catalysts can be added to the soaker drum via line 19.
  • Steam, C minus, air, or a mixture thereof, can also be used in the soaker drum to increase reaction rates, strip lower boiling components, and to keep the solids suspended in a slurry.
  • the soaker drum may be continuously cleaned by mechanical means to minimize coke deposits.
  • the soaker drum is operated at effective temperatures and residence times to initiate coking reactions, but not to the extent that coke deposits significantly build-up in the soaker drum.
  • Preferred conditions include temperatures from about 350°C to about 520°C, preferably from about 400°C to about 450°C and residence times of from about 1 to 60 minutes, preferably from about 5 to 30 minutes, depending on the feed properties and desired feed decontamination rates.
  • Proper use of the soaker drum will selectively condense only the highest boiling vapor products and produce a pre-polymerized heavy oil which is recycled to reaction zone I via line 9. This will result in an increased metals rejection rate from about 90% for once-through to 95% or greater with extinction recycle.
  • Use of the soaker drum also enables increased rejection of other feed contaminants, such as Conradson Carbon, sulfur, and nitrogen.
  • the resulting liquid product quality is substantially improved and of higher value as feed to refinery conversion processes.
  • the vapor fraction from soaker drum 2 is passed via line 14 to cyclone 20 where most of the entrained solids, or dust, are removed.
  • the dedusted vapors are then passed to quench zone 13 via line 24 where the vapors are reduced to temperatures below which substantial thermal cracking occurs. This temperature will preferably be below about 450°C, more preferably below about 340°C.
  • Solids, having carbonaceous material deposited thereon, are passed from reaction zone 1 via line 15 to the bed of solids 17 in stripper 3.
  • the solids pass downwardly through the stripper and past a stripping zone at the bottom section where any remaining volatiles, or vaporizable material, are stripped from the solids with use of a stripping gas, preferably steam, introduced into the stripping zone via line 16.
  • a stripping gas preferably steam
  • Stripped vapor products pass upwardly in stripper vessel 3 to quench zone 13 where a light product is removed overhead via line 28.
  • the light product will typically be a 550°C minus product stream.
  • a 550°C plus stream will also be collected from the quench zone via line 26.
  • the stripped solids are passed via line 18 to heater 4 which contains a heating zone.
  • the heating zone is operated in an oxidizing gas environment, preferably air, at an effective temperature. That is, at a temperature that will meet the heat requirements of the reaction zone.
  • the heating zone will typically be operated at a temperature of about 40°C to 200°C, preferably from about 50°C to 175°C, more preferably from about 50°C to 120°C in excess of the operating temperature of reaction zone 1.
  • preheated air can be introduced into the heater. While some carbonaceous residue will be burned from the solids in the heating zone, it is preferred that only partial combustion take place so that the solids, after passing through the heater, will have value as a fuel.
  • Excess solids can be removed from the process unit via line 50. Flue gas is removed overhead from heater 4 via line 40. The flue gas is passed through a cyclone system 36, 39, and 38 to remove most solid fines. Dedusted flue gas will be passed to a co-boiler for waste heat recovery (not shown), scrubbed to remove contaminants and particulates, and passed to atmosphere. The hot inert solids are then recycled via lines 12 to thermal zonel.

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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)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Working-Up Tar And Pitch (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

On fait passer le flux en phase vapeur via la canalisation (11) dans une machine à tambour (2) maintenue en conditions efficaces de sorte que les matériaux au point d'ébullition les plus élevés se condensent. En règle générale, ces conditions ont trait au refroidissement contrôlé de la fraction vapeur juste en dessous du point de rosée. On peut également faire passer un flux de refroidissement dans le tambour par la canalisation (21).
PCT/US2000/009607 1999-04-16 2000-04-11 Procede ameliore de desasphaltage de residus faisant appel a un recyclage reactif d'une matiere a point d'ebullition eleve WO2000063320A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP00925922.7A EP1194498B1 (fr) 1999-04-16 2000-04-11 Procede ameliore de desasphaltage de residus faisant appel a un recyclage reactif d'une matiere a point d'ebullition eleve
AU44542/00A AU771590B2 (en) 1999-04-16 2000-04-11 Improved process for deasphalting residua by reactive recycle of high boiling material
ES00925922.7T ES2559272T3 (es) 1999-04-16 2000-04-11 Proceso mejorado para desasfaltar residuos por reciclado reactivo de material de alto punto de ebullición
CA2370591A CA2370591C (fr) 1999-04-16 2000-04-11 Procede ameliore de desasphaltage de residus faisant appel a un recyclage reactif d'une matiere a point d'ebullition eleve
JP2000612401A JP4590108B2 (ja) 1999-04-16 2000-04-11 高沸点物質の反応再循環による残油の改良された脱歴方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US29302999A 1999-04-16 1999-04-16
US09/293,029 1999-04-16

Publications (1)

Publication Number Publication Date
WO2000063320A1 true WO2000063320A1 (fr) 2000-10-26

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Country Status (8)

Country Link
EP (1) EP1194498B1 (fr)
JP (1) JP4590108B2 (fr)
CN (1) CN1347442A (fr)
AR (1) AR023503A1 (fr)
AU (1) AU771590B2 (fr)
CA (1) CA2370591C (fr)
ES (1) ES2559272T3 (fr)
WO (1) WO2000063320A1 (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003085069A1 (fr) * 2002-04-01 2003-10-16 Exxonmobil Research And Engineering Company Procede de conversion de residus ameliore
US7419585B2 (en) 2000-05-01 2008-09-02 Exxonmobil Research And Engineering Company Process for upgrading residua
KR20190017824A (ko) * 2016-06-14 2019-02-20 스톤, 리차드 난류 중간상 피치 공정 및 제품
WO2019055305A1 (fr) * 2017-09-12 2019-03-21 Saudi Arabian Oil Company Processus intégré de production de brai et de pétrochimie de mésophase
US10508240B2 (en) 2017-06-19 2019-12-17 Saudi Arabian Oil Company Integrated thermal processing for mesophase pitch production, asphaltene removal, and crude oil and residue upgrading
US10913901B2 (en) 2017-09-12 2021-02-09 Saudi Arabian Oil Company Integrated process for mesophase pitch and petrochemical production
KR20220021177A (ko) * 2020-08-13 2022-02-22 최창균 피치 개질장치 의 원료피치 연속 공급 및 개질된 피치 연속 배출

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5239226B2 (ja) * 2007-06-28 2013-07-17 株式会社Ｉｈｉ 重質燃料の改質方法及びその改質装置
DE102018213210A1 (de) 2018-08-07 2020-02-13 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur Reinigung mineralischer Feststoffe und Holzmaterialien, Vorrichtung für dieses Verfahren und deren Verwendung

Citations (4)

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Publication number Priority date Publication date Assignee Title
US3334043A (en) * 1965-09-29 1967-08-01 Sun Oil Co Neopentane separation of bituminous materials
US4054512A (en) * 1976-10-22 1977-10-18 Exxon Research And Engineering Company Deasphalting with liquid hydrogen sulfide
US4191639A (en) * 1978-07-31 1980-03-04 Mobil Oil Corporation Process for deasphalting hydrocarbon oils
US5714056A (en) * 1995-07-17 1998-02-03 Exxon Research And Engineering Company Process for deasphalting residua (HEN9511)

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4277324A (en) * 1979-04-13 1981-07-07 Exxon Research & Engineering Co. Treatment of pitches in carbon artifact manufacture

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3334043A (en) * 1965-09-29 1967-08-01 Sun Oil Co Neopentane separation of bituminous materials
US4054512A (en) * 1976-10-22 1977-10-18 Exxon Research And Engineering Company Deasphalting with liquid hydrogen sulfide
US4191639A (en) * 1978-07-31 1980-03-04 Mobil Oil Corporation Process for deasphalting hydrocarbon oils
US5714056A (en) * 1995-07-17 1998-02-03 Exxon Research And Engineering Company Process for deasphalting residua (HEN9511)

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP1194498A4 *

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7419585B2 (en) 2000-05-01 2008-09-02 Exxonmobil Research And Engineering Company Process for upgrading residua
WO2003085069A1 (fr) * 2002-04-01 2003-10-16 Exxonmobil Research And Engineering Company Procede de conversion de residus ameliore
US7033486B2 (en) 2002-04-01 2006-04-25 Exxonmobil Research And Engineering Company Residuum conversion process
KR20190017824A (ko) * 2016-06-14 2019-02-20 스톤, 리차드 난류 중간상 피치 공정 및 제품
KR102604852B1 (ko) 2016-06-14 2023-11-21 에이씨피 테크놀로지스, 엘엘씨 난류 중간상 피치 공정 및 제품
US10508240B2 (en) 2017-06-19 2019-12-17 Saudi Arabian Oil Company Integrated thermal processing for mesophase pitch production, asphaltene removal, and crude oil and residue upgrading
KR20200052364A (ko) * 2017-09-12 2020-05-14 사우디 아라비안 오일 컴퍼니 중간상 피치 및 석유화학 제품 생산을 위한 통합된 공정
US10913901B2 (en) 2017-09-12 2021-02-09 Saudi Arabian Oil Company Integrated process for mesophase pitch and petrochemical production
KR102355405B1 (ko) * 2017-09-12 2022-02-08 사우디 아라비안 오일 컴퍼니 중간상 피치 및 석유화학 제품 생산을 위한 통합된 공정
US11319490B2 (en) 2017-09-12 2022-05-03 Saudi Arabian Oil Company Integrated process for mesophase pitch and petrochemical production
WO2019055305A1 (fr) * 2017-09-12 2019-03-21 Saudi Arabian Oil Company Processus intégré de production de brai et de pétrochimie de mésophase
KR20220021177A (ko) * 2020-08-13 2022-02-22 최창균 피치 개질장치 의 원료피치 연속 공급 및 개질된 피치 연속 배출
KR102481197B1 (ko) * 2020-08-13 2022-12-27 최창균 원료피치의 연속 공급 및 개질된 전구체피치의 연속 배출이 가능한 피치 개질수단 및 연속개질장치

Also Published As

Publication number Publication date
CA2370591A1 (fr) 2000-10-26
CA2370591C (fr) 2011-01-11
EP1194498B1 (fr) 2015-11-11
JP4590108B2 (ja) 2010-12-01
ES2559272T3 (es) 2016-02-11
AU771590B2 (en) 2004-03-25
AU4454200A (en) 2000-11-02
CN1347442A (zh) 2002-05-01
EP1194498A4 (fr) 2011-02-16
JP2002542375A (ja) 2002-12-10
AR023503A1 (es) 2002-09-04
EP1194498A1 (fr) 2002-04-10

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