EP0287796A1 - Procédé pour l'hydroconversion des huiles lourdes et des huiles résiduelles - Google Patents

Procédé pour l'hydroconversion des huiles lourdes et des huiles résiduelles Download PDF

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Publication number
EP0287796A1
EP0287796A1 EP19880103755 EP88103755A EP0287796A1 EP 0287796 A1 EP0287796 A1 EP 0287796A1 EP 19880103755 EP19880103755 EP 19880103755 EP 88103755 A EP88103755 A EP 88103755A EP 0287796 A1 EP0287796 A1 EP 0287796A1
Authority
EP
European Patent Office
Prior art keywords
oils
waste
additive
heavy
coal
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.)
Granted
Application number
EP19880103755
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German (de)
English (en)
Other versions
EP0287796B1 (fr
Inventor
Ludwig Dr. Merz
Klaus Dr. Niemann
Klaus Kretschmer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Veba Oel Technologie und Automatisierung GmbH
Original Assignee
Veba Oel Technologie und Automatisierung GmbH
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.)
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Publication date
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Publication of EP0287796A1 publication Critical patent/EP0287796A1/fr
Application granted granted Critical
Publication of EP0287796B1 publication Critical patent/EP0287796B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/08—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts
    • C10G1/083—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts in the presence of a solvent
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G49/00—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00
    • C10G49/10—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 with moving solid particles
    • C10G49/12—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 with moving solid particles suspended in the oil, e.g. slurries

Definitions

  • the older patent application P 3634275.0 describes a process for the hydrogenating conversion of heavy and residual oils, waste and waste oils and, if appropriate, their mixtures with ground brown and hard coal in the sump or combined sump and gas phase with hydrogen-containing gases at a hydrogen partial pressure from 50 to 300 bar, preferably 150 to 200 bar, a temperature of 250 to 500 ° C, preferably 400 to 490 ° C, a gas-oil ratio of 100 to 10,000 Nm3 / t, preferably 1,000 to 5,000 Nm3 / t of liquid and solid feed products with the addition of at least one additive in quantities of 0.5 to 5.0% by weight, based on the total amount of liquid and solid feed products, and for the purpose of increasing the specific throughput of the bottom phase reactors, the additive is added in two different particle size ranges.
  • the components can also advantageously be used in the weight ratio a) + b) to c) from 100: 1 to 1: 1.5.
  • sewage sludge from primary settling tanks, biological clarification, digestion towers, paint sludge, halogen-containing solvents or their distillation residues or from recycling processes PCB-containing or halogen-containing waste oils, which can also contain solids, transformer oils, hydraulic oils, organic residues Chemical cleaning companies, organic residues from part degreasing or cleaning baths, landfill leachate oils, bilge oils, tank cleaning residues, plastics or waste plastics from pressure hydrogenation under the typical conditions of a sump phase hydrogenation in a cascade of sump phase hydrogenation reactors or in a single hydrogenation reactor with one or more downstream hot separators or a combined bottom phase gas phase hydrogenation.
  • the heat of hydrogenation that is generated during the conversion of the heavy oils is used for the conversion and decontamination of the waste oils or waste materials under the conditions of the phase of hydrogenation.
  • the hydrating treatment of such waste oils or waste materials only a slight exotherm is normally to be expected. This significantly reduces the load on the preheater system of a typical sump phase hydrogenation system.
  • the bubble column maintained in the hydrogenation reactors during operation is suitable for processing waste oils containing solids as well, by using the stable fluid dynamics of the mixture of residual oil or heavy oil based on mineral oil with the hydrogenation gas as a "supporting" component.
  • waste oils or waste materials that are classified as hazardous waste can be disposed of in such a way that the carbon-containing constituents contained in these substances, hydrocarbon chains in particular are retained.
  • heteroatoms in particular oxygen, sulfur, nitrogen and halogens
  • oxygen, sulfur, nitrogen and halogens are largely removed by conversion into the corresponding hydrogen compounds, transition into the gas phase and their discharge with the waste water, in which the hydrogen halides and ammonia and hydrogen sulfide dissolve in whole or in part.
  • the contents of heavy metals or ash-forming constituents in the feed materials are effectively transferred to the residue in the hot separator systems following the bottom phase hydrogenation.
  • the amounts involved are different, for example, in the case of waste oils or sewage sludge containing solids, increased amounts of ash formers and heavy metals have to be discharged via the residue.
  • the feedstocks mentioned, which form the condensed phase can also be used with coal in a weight ratio of 20: 1 to 1: 1.5, preferably 5: 1 to 5: 4.
  • an additive in the form of a carbon-containing, surface-rich suspended solid is used in the bottom phase hydrogenation in amounts of 0.1 to 10, preferably 0.5 to 5.0,% by weight preferred to use lignite coke from shaft and hearth furnaces, soot from the gasification of heavy oil, hard coal, hydrogenation residues or lignite and the activated coke, petroleum coke and dusts from the Winkler gasification of coal produced therefrom.
  • the carbon-containing additives used can advantageously be impregnated with solutions of metal salts, of metals from the 1st to 8th subgroup and the 4th main group of the periodic system of the elements, preferably iron, cobalt, nickel, vanadium or molybdenum.
  • carbon-containing, surface-rich additives to the bottom phase hydrogenation also favors reactions of hydrodemetallization and hydrodesulfurization, which lead to the removal of the metal-containing or ash-forming constituents with the hot separator residue.
  • these components are brought into a state that is easier to handle than in the starting material.
  • these components are so far enriched in the hot separator residue that they can also be recovered, for example, by metallurgical processes.
  • the additive in two fractions that are sharply separated according to the grain spectrum, but it can also be used in a continuous grain size distribution with the corresponding large grain fraction of 100 ⁇ m or larger.
  • a sewage sludge In the hydrogenation of mixtures of heavy or residual oils, waste or waste oils with sewage sludge, the weight ratio of oil to sewage sludge being preferably from 10: 1 to 1: 1.5, a sewage sludge can be used which has a corresponding proportion of coarse grain fraction of 100 ⁇ m or larger contains.
  • the sewage sludge can replace all or part of the additive.
  • the proportion of the coarse grain fraction can be 20% by weight or more of the additive added, which should include both carbon-containing, surface-rich, suspended solids and the aforementioned red masses, iron oxides, electrostatic filter dust and cyclone dust.
  • weight ratios of oil to coal from 5: 1 to 1: 1.5 are advantageous, with a proportion of the coal in grain sizes of 100 corresponding to the proportion of the coarse grain fraction of the additive to be added ⁇ m or larger can be used.
  • neutralizing agents which is necessary due to the halogen constituents of the waste oils or waste materials used to neutralize the hydrogen halides formed, is preferably carried out in amounts of 0.01 to 5.0% by weight of compounds which salts with hydrogen halide by neutralization form or split off hydroxide ions in aqueous solution.
  • the compounds to be added for this purpose are preferably injected together with water at a suitable point into the effluent from the bottom phase reactor and can be discharged from the process in the so-called cold separators as an aqueous solution of the corresponding halides, for example by phase separation.
  • sodium sulfide in the form of the aqueous solution, in suspension with oils or the like, as a compound which forms salts with hydrogen halide by neutralization or which releases hydroxide ions in aqueous solution.
  • sewage sludge as a preferred embodiment of the present process, it is expedient to dry to a water content of less than 10.0% by weight, preferably less than 2.0% by weight and, if necessary, by grinding, sieving and / or screening processes from coarse foreign bodies and brought to a grain size of less than 1.0 mm, preferably less than 0.5 mm.
  • the sewage sludge treated in this way can completely or partially replace an added disposable additive.
  • the disposable additive is selected depending on the desired conversion rate and the tendency of the feed material to form coke, according to the type and amount added.
  • the present process for the hydrogenative conversion of heavy and residual oils, in a mixture with municipal or industrial sewage sludge in the bottom or combined bottom and gas phase is expediently carried out in such a way that a high-pressure pump contains the oil or the oil / solid mixture including the additive in the high pressure part of the system.
  • Hydrogen-containing cycle gas and fresh hydrogen are heated and mixed, for example, with the residual oil in the high pressure section.
  • the reaction mixture flows through a regenerator battery and a peak heater to utilize the heat of reaction of the reaction products and then reaches the bottom phase reactors.
  • the reactor system consists, for example, of three vertical empty tube reactors connected in series, which are fed with the flow direction from bottom to top.
  • the conversion takes place at temperatures between preferably 400 to 490 ° C and a hydrogen partial pressure of 50 to 350 bar.
  • a quasi-isothermal mode of operation of the reactors is possible by feeding in cold gas.
  • downstream hot separators which are operated at approximately the same temperature level as the reactors, the unconverted portion of the heavy and residual oils used as well as the solids is separated from the gaseous reaction products under process conditions.
  • the bottom product of the hot separators is expanded in a multi-stage flash unit.
  • the top product of the hot separator, the flash distillates and any crude oil distillate fractions to be processed are combined and fed to the downstream gas phase reactors.
  • Hydrotreating or even mild hydrocracking is carried out on a catalytic fixed bed, for example under what are known as trickle flow conditions, under preferably the same total pressure as in the bottom phase.
  • gas and liquid are separated in a high-pressure cold separator. After phase separation, the wastewater can be discharged from the process at this point.
  • the liquid product is decompressed and processed in standard refinery processes.
  • the gaseous reaction products (C1 to C4 gases, H2S, NH3, hydrogen halides) accumulate in the process gas, the water-soluble components with the waste water and the C1 to C4 gases depending on their solubility are expediently removed in an oil wash.
  • the hydrogen remaining in the process gas with small amounts of inert gases and other gaseous constituents is recycled as recycle gas.
  • a vacuum residue from Middle East crude oil is mixed with 15% by weight of a used industrial cleaning solution with a chlorine content of 4% by weight and 15% by weight sewage sludge (dried to less than 2% by weight). -% residual moisture) with 1.5 m3 H2 per kg of mash used at 210 bar hydrogen partial pressure.
  • the sewage sludge was ground in such a way that 90% of the material in the grain spectrum was smaller than 90 ⁇ m and 10% between 100 and 150 ⁇ m.
  • Na2S based on the mash was metered in continuously.
  • the vacuum residue was converted to 91% by weight into low-boiling products. These products contain less than 1 wt .-% ppm chlorine, the organic part of the sewage sludge is more than 75 wt .-% in liquid Products implemented. A hydrocarbon gas formation (C1 - C4) of 8.1 wt .-% based on the mash used was observed.
  • a Venezuelan vacuum residue is reacted together with 30% by weight (based on vacuum residue) of a used metal degreasing solution.
  • the aromatic and phenol-containing degreasing solution has a chlorine content of 1.02% by weight and an oxygen content of 3.7% by weight, nitrogen of 0.92% by weight and sulfur of 0.98% by weight.
  • the proportion boiling below 200 ° C is 44% by weight
  • the proportion of the fraction 200 to 350 ° C is 22% by weight.
  • the reaction in the bottom phase hydrogenation is carried out with the addition of 2% by weight of a brown coal coke as an additive with particle sizes of 1.5% by weight less than 90 ⁇ m and 0.5% by weight from 100 to 400 ⁇ m with a specific throughput of 0.5 kg / lh (based on vacuum residue), an H2 / oil ratio of 2000 Nm3 / t and a hydrogen partial pressure of 200 bar.
  • the vacuum residue used was converted to 90% by weight into low-boiling products (less than 500 ° C).
  • the primary product of the bottom phase hydrogenation has a chlorine content of less than 1% by weight ppm.
  • the chlorine contained in the metal degreasing solution becomes sodium chloride with a Hot separator solid discharged.
  • the primary product of the bottom phase hydrogenation is subjected to a catalytic fixed bed refining in a commercially available refining contact in the directly coupled gas phase hydrogenation at 380 ° C and a catalyst load of 2.0 kg / kg.h.
  • the total product produced after the gas phase hydrogenation is phenol-free and free of chlorine, the sulfur and nitrogen content is less than 0.1% by weight.
  • a Venezuelan vacuum residue is dried together with 10% by weight of a distillation residue from solvent recycling (at 100 ° C. in a vacuum, ground and sieved to less than 150 ⁇ m, of which 75% by weight) Particle size less than 90 and 25 wt .-% have a particle size of 100 to 150 microns) with a specific throughput of 0.5 kg mash / lh, an H2 / oil ratio of 3000 Nm3 / t and a hydrogen partial pressure of 200 bar implemented.
  • the vacuum residue used is converted to 94% by weight into low-boiling products.
  • the organic fraction of the distillation residue (ash content: 17% by weight, carbon content: 54% by weight, hydrogen content: 6.5% by weight, sulfur content: 0.2% by weight, balance: nitrogen and oxygen) becomes over 80% by weight converted into liquid products and gases.

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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)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Treatment Of Sludge (AREA)
  • Catalysts (AREA)
  • Fats And Perfumes (AREA)
  • Processing Of Solid Wastes (AREA)
EP88103755A 1987-03-30 1988-03-10 Procédé pour l'hydroconversion des huiles lourdes et des huiles résiduelles Expired - Lifetime EP0287796B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3710021 1987-03-30
DE19873710021 DE3710021A1 (de) 1987-03-30 1987-03-30 Verfahren zur hydrierenden konversion von schwer- und rueckstandsoelen

Publications (2)

Publication Number Publication Date
EP0287796A1 true EP0287796A1 (fr) 1988-10-26
EP0287796B1 EP0287796B1 (fr) 1995-12-06

Family

ID=6324069

Family Applications (1)

Application Number Title Priority Date Filing Date
EP88103755A Expired - Lifetime EP0287796B1 (fr) 1987-03-30 1988-03-10 Procédé pour l'hydroconversion des huiles lourdes et des huiles résiduelles

Country Status (11)

Country Link
US (1) US4941966A (fr)
EP (1) EP0287796B1 (fr)
JP (1) JPS63260984A (fr)
AT (1) ATE131203T1 (fr)
CA (1) CA1304310C (fr)
DD (1) DD268477A5 (fr)
DE (2) DE3710021A1 (fr)
ES (1) ES2081283T3 (fr)
GR (1) GR3018806T3 (fr)
NO (1) NO174933C (fr)
RU (1) RU1836408C (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0314992A3 (fr) * 1987-11-04 1990-01-17 VEBA OEL Entwicklungs-Gesellschaft mbH Procédé d'hydroconversion d'huiles lourdes, d'huiles résiduelles et d'huiles usées en mélange avec des boues d'épuration

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US5166118A (en) * 1986-10-08 1992-11-24 Veba Oel Technologie Gmbh Catalyst for the hydrogenation of hydrocarbon material
US5374348A (en) * 1993-09-13 1994-12-20 Energy Mines & Resources - Canada Hydrocracking of heavy hydrocarbon oils with heavy hydrocarbon recycle
US5849172A (en) * 1997-06-25 1998-12-15 Asarco Incorporated Copper solvent extraction and electrowinning process
US5904838A (en) * 1998-04-17 1999-05-18 Uop Llc Process for the simultaneous conversion of waste lubricating oil and pyrolysis oil derived from organic waste to produce a synthetic crude oil
US7444305B2 (en) * 2001-02-15 2008-10-28 Mass Connections, Inc. Methods of coordinating products and service demonstrations
US7745369B2 (en) 2003-12-19 2010-06-29 Shell Oil Company Method and catalyst for producing a crude product with minimal hydrogen uptake
US7763160B2 (en) 2003-12-19 2010-07-27 Shell Oil Company Systems and methods of producing a crude product
US7591941B2 (en) 2003-12-19 2009-09-22 Shell Oil Company Systems, methods, and catalysts for producing a crude product
TW200602591A (en) * 2004-07-08 2006-01-16 hong-yang Chen Gas supply device by gasifying burnable liquid
US7918992B2 (en) 2005-04-11 2011-04-05 Shell Oil Company Systems, methods, and catalysts for producing a crude product
BRPI0609416A2 (pt) 2005-04-11 2011-10-11 Shell Int Research método para produzir um produto bruto
US20080083655A1 (en) 2006-10-06 2008-04-10 Bhan Opinder K Methods of producing a crude product
TW201026837A (en) * 2008-09-17 2010-07-16 Bdi Bio Diesel Internat Ag Process for obtaining combustibles and fuels, respectively
US9168506B2 (en) 2010-01-21 2015-10-27 Intevep, S.A. Additive for hydroconversion process and method for making and using same
GB2478332A (en) 2010-03-04 2011-09-07 Grimley Smith Associates Method of metals recovery from refinery residues
US8999145B2 (en) 2012-10-15 2015-04-07 Uop Llc Slurry hydrocracking process
US9951282B2 (en) 2013-03-14 2018-04-24 Bp Europa Se Process for introducing fine and coarse additives for hydroconversion of heavy hydrocarbons
US10745629B2 (en) 2017-01-16 2020-08-18 Council Of Scientific And Industrial Research Process for upgradation of heavy crude oil/residue using waste plastic as hydrogen donating agent
IT201800020818A1 (it) * 2018-12-21 2020-06-21 Eni Spa Procedimento di idroconversione di miscele di polimeri
CN111909719A (zh) * 2020-06-19 2020-11-10 张家港保税区慧鑫化工科技有限公司 一种重油多产石脑油的生产系统及生产方法
CN111849554A (zh) * 2020-07-03 2020-10-30 张家港保税区慧鑫化工科技有限公司 一种垃圾液相悬浮床加氢处理系统及工艺
CN111808636A (zh) * 2020-07-17 2020-10-23 张家港保税区慧鑫化工科技有限公司 一种污泥重油处理方法
CN111808632A (zh) * 2020-07-17 2020-10-23 张家港保税区慧鑫化工科技有限公司 一种油和有机废物混合物的加工方法
CN111849555A (zh) * 2020-07-21 2020-10-30 张家港保税区慧鑫化工科技有限公司 一种加氢处理含卤素废油的系统及方法
US12441668B2 (en) * 2020-12-28 2025-10-14 Sabic Global Technologies B.V. Method of processing waste plastic and pyrolysis oil from waste plastic
EP4032963A1 (fr) 2021-01-21 2022-07-27 Basell Poliolefine Italia S.r.l. Procédé d'hydrodépolymérisation de déchets polymères

Citations (1)

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EP0182309A1 (fr) * 1984-11-22 1986-05-28 RWE Entsorgung Aktiengesellschaft Procédé pour la réutilisation par hydration de déchets contenant du carbone d'origine synthétique

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0314992A3 (fr) * 1987-11-04 1990-01-17 VEBA OEL Entwicklungs-Gesellschaft mbH Procédé d'hydroconversion d'huiles lourdes, d'huiles résiduelles et d'huiles usées en mélange avec des boues d'épuration

Also Published As

Publication number Publication date
ES2081283T3 (es) 1996-03-01
EP0287796B1 (fr) 1995-12-06
CA1304310C (fr) 1992-06-30
NO881408L (no) 1988-10-03
NO881408D0 (no) 1988-03-29
NO174933B (no) 1994-04-25
GR3018806T3 (en) 1996-04-30
DE3710021A1 (de) 1988-10-20
NO174933C (no) 1994-08-03
ATE131203T1 (de) 1995-12-15
DE3854747D1 (de) 1996-01-18
JPS63260984A (ja) 1988-10-27
US4941966A (en) 1990-07-17
DD268477A5 (de) 1989-05-31
RU1836408C (ru) 1993-08-23

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