EP0287796B1 - 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
EP0287796B1
EP0287796B1 EP88103755A EP88103755A EP0287796B1 EP 0287796 B1 EP0287796 B1 EP 0287796B1 EP 88103755 A EP88103755 A EP 88103755A EP 88103755 A EP88103755 A EP 88103755A EP 0287796 B1 EP0287796 B1 EP 0287796B1
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Prior art keywords
weight
oils
process according
solid
heavy
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Expired - Lifetime
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EP88103755A
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German (de)
English (en)
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EP0287796A1 (fr
Inventor
Ludwig Dr. Merz
Klaus Dr. Niemann
Klaus Kretschmer
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Veba Oel Technologie und Automatisierung GmbH
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Veba Oel Technologie und Automatisierung GmbH
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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

  • EP-A-0 263 522 with its priority DE-A 3634275.0 describes a process for the hydrogenative 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 bottom and gas phase with hydrogen-containing gases at a hydrogen partial pressure of 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 liquid and solid feed products with addition of at least one additive in amounts of 0.5 to 5.0 wt .-% based on the total amount of liquid and solid feed products proposed and in order to increase the specific throughput of the bottom phase reactors added in two different grain size ranges.
  • the invention relates to a.
  • the present method of admixing waste oils or waste materials, ie organic or synthetic, uncrosslinked or also crosslinked Substances containing carbon chains to the feed stream of hydrogenation systems consisting, for example, of residual oil, heavy oil or vacuum residue or admixture as a side stream into the hydrogenation reactor have the following advantages.
  • 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-phase 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 components contained in these substances, hydrocarbon chains in particular are retained.
  • heteroatoms in particular 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 feed materials 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.
  • the carbon-containing solids used with two grain size ranges can advantageously be impregnated with solutions of metal salts, of metals from subgroups 1 to 8 and the fourth main group of the periodic system of the elements, preferably iron, cobalt, nickel, vanadium or molybdenum.
  • the solid with two grain size ranges in two fractions which are sharply separated according to the grain spectrum, but it can also be used in a continuous grain size distribution with the corresponding coarse 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.
  • the proportion of the coarse grain fraction can be 20% by weight or more of the added solid with two grain size ranges, this being understood to mean 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 part of the coal corresponding to the proportion of the coarse grain fraction of the solid to be added with two grain size ranges Grain sizes of 100 »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 in 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 the 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 advisable 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 acts as a solid with two grain size ranges.
  • the added solid with two grain size ranges is selected according to 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 also 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 Solids with two grain size ranges in the high pressure part of the plant.
  • Hydrogen-containing cycle gas and fresh hydrogen are heated up 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 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 separator is expanded in a multi-stage flash unit.
  • the top product of the hot separators, the flash distillates and any crude oil distillate fractions to be processed are combined and fed to the downstream gas phase reactors.
  • Hydrotreating or 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 are expediently discharged in an oil wash according to their solubility.
  • 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 less than 90 »m and 10% between 100 and 150» m.
  • To incorporate the chlorine 1% by weight Na2S based on the mash was metered in continuously. At 465 ° C.
  • 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 Venezuelan vacuum residue is reacted together with 30% by weight (based on vacuum residue), corresponding to 22.7% by weight based on the total mash used, of a used metal degreasing solution.
  • the aromatic and phenol-containing degreasing solution has a chlorine content of 1.02% by weight and oxygen contents of 3.7% by weight, nitrogen of 0.92% by weight and sulfur of 0.98% by weight.
  • the fraction boiling below 200 ° C is 44% by weight
  • the fraction 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 with grain 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 together with 10% by weight of a distillation residue from solvent recycling (dried at 100 ° C. in vacuo, ground and sieved to less than 150 »m, of which 75% by weight a particle size less than 90 and 25 wt .-% have a particle size of 100 to 150 »m) 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.
  • 94% by weight of the vacuum residue used is converted 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)

Claims (13)

  1. Procédé de conversion hydrogénante de :
    - huiles lourdes et huiles résiduelles,
    - huiles usées et huiles de rebut,
       ainsi que le cas échéant des mélanges avec du lignite et de la houille concassés,
       en phase liquide ou en phase combinée liquide/gaz avec des gaz contenant de l'hydrogène à,
    - une pression partielle d'hydrogène de 50 à 350 bars, de préférence de 150 à 200 bars,
    - une température de 250 à 500°C, de préférence 400 à 490°C,
    - un rapport gaz/huile de 100 à 10000 Nm³/t de préférence 1000 à 5000 Nm³/t de produits d'utilisation liquides et solides,
       caractérisé en ce que l'on met en oeuvre :
       au moins une matière solide en quantités de 0,1 à 15 % en poids, rapporté à la quantité totale de produits d'utilisation liquides et solides, et ayant les plages de tailles de grains :
    - 90 »m ou moins,
    - et 100 »m à 1000 »m, de préférence 100 à 500 »m,
       qui se présentent respectivement soit à l'intérieur d'une distribution continue de tailles de grains soit, de préférence en tant que deux fractions nettement séparées,
       et des mélanges de :
    a) huiles lourdes ou huiles résiduelles,
    b) huiles usées et huiles de rebut principalement,
    - des huiles usées contenant du PCB ou contenant des halogènes qui peuvent aussi contenir des matières solides,
    - des huiles de transformateur,
    - des huiles hydrauliques,
    - des huiles d'infiltration des dépotoirs,
    - des huiles de fond de cale
    - des boues d'épuration provenant :
    - de pré-bassins d'épuration,
    - d'épuration biologique,
    - des tours de pourrissement,
    - des boues de laques,
    - de solvants contenant des halogènes,
    - de résidus organiques provenant d'entreprises de nettoyage chimique, dégraissage de pièces,
    - bains de nettoyage,
    - nettoyage des réservoirs,
    - distillation de solvants halogénés,
       ou à partir de processus de recyclage ou des matières plastiques, des matières plastiques usagées, des déchets de production de matière plastique,
       à un débit de 0,1 à 2 t/m³/h, rapporté à l'huile lourde ou à l'huile résiduelle, et à un rapport pondéral de 100 : 1 à 1 : 1,5.
  2. Procédé selon la revendication 1, caractérisé en ce que le charbon et les substances d'utilisation habituelles sont mis en oeuvre dans un rapport pondéral de 1 : 20 à 1,5, de préférence 1 : 5 à 4 : 5.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce qu'une quantité qui doit être ajoutée, de la fraction de grains grossiers de la matière solide, ayant deux plages de tailles de grains est mise en oeuvre avec la partie correspondante du charbon en tailles de grains de 100 »m ou plus grand.
  4. Procédé selon au moins une des revendications précédentes, caractérisé en ce que l'on utilise dans l'hydrogénation en phase liquide, de 0,5 à 5,0 % en poids d'une matière solide mise en suspension contenant du carbone, riche en surfaces ayant deux plages de tailles de grains.
  5. Procédé selon au moins une des revendications précédentes, caractérisé en ce que comme matière solide, ayant deux plages de tailles de grains, du coke de lignite, provenant des fourneaux de mine et de fourneaux de cuisinière, du noir de fumée provenant de la gazéification d'huiles lourdes, de la houille, des résidus d'hydrogénation ou du lignite et les cokes actifs, les cokes de pétrole obtenus à partir de cela, les poussières provenant de la gazéification de Winkler du charbon, trouvent une utilisation.
  6. Procédé selon au moins une des revendications précédentes, caractérisé en ce que les matières solides contenant du carbone, mises en jeu avec deux plages de tailles de grains sont imprégnées de solutions de sels métalliques du 1er au 8ème sous groupe ainsi que du 4ème groupe principal du système périodique des éléments, de préférence le fer, le cobalt, le nickel, le vanadium et le molybdène.
  7. Procédé selon au moins une des revendications 1 à 3, caractérisé en ce que comme matière solide, ayant deux plages de tailles de grains, on met en oeuvre de 0,5 à 5,0 % en poids de masse rouge, d'oxyde de fer, de poussières d'électrofiltration, et de poussières de cyclone provenant du traitement des minerais de métal.
  8. Procédé selon au moins une des revendications précédentes, caractérisé en ce que la quantité de la proportion de grains grossiers s'élève à 20 % en poids ou plus de la matière solide ajoutée, ayant deux plages de tailles de grains.
  9. Procédé selon au moins une des revendications précédentes, caractérisé en ce que l'on ajoute 0,01 à 5,0 % en poids d'un composé qui forme des sels par neutralisation avec un acide halohydrique, ou détache en solution aqueuse des ions hydroxydes, conjointement avec des produits d'utilisation.
  10. Procédé selon la revendication 9, caractérisé en ce que le composé qui forme des sels par neutralisation avec un acide halohydrique, ou détache en solution aqueuse des ions hydroxydes est injecté conjointement avec l'eau dans le courant d'efflux du réacteur en phase liquide.
  11. Procédé selon la revendication 9 ou la revendication 10, caractérisé en ce que l'on ajoute de 0,01 à 5,0 % en poids de SNa₂.
  12. Procédé selon au mois une des revendications précédentes, caractérisé en ce que lors de l'hydrogénation de mélanges à base d'huiles lourdes et d'huiles résiduelles, d'huiles usées et d'huiles de rebut avec des boues d'épuration, pour lesquels le rapport pondéral huile pour boue d'épuration s'élève de 10 : 1 à 1 : 1,5, on met en oeuvre une boue d'épuration qui contient une proportion correspondante en fraction de grains grossiers de 100 »m ou plus grand.
  13. Procédé selon la revendication 12, caractérisé en ce que la boue d'épuration mise en jeu est séchée jusqu'à une teneur en eau de moins de 10,0, de préférence moindre que 2,0 % en poids, et que l'on débarrasse par des processus de broyage, de tamisage et/ou de criblage des solides étrangers grossiers et que l'on amène à une granulation de moins de 1,0, de préférence de moins de 0,5 mm.
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 EP0287796A1 (fr) 1988-10-26
EP0287796B1 true EP0287796B1 (fr) 1995-12-06

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EP88103755A Expired - Lifetime EP0287796B1 (fr) 1987-03-30 1988-03-10 Procédé pour l'hydroconversion des huiles lourdes et des huiles résiduelles

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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)

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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
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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
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US4370221A (en) * 1981-03-03 1983-01-25 Her Majesty The Queen In Right Of Canada, As Represented By The Minister Of Energy, Mines And Resources Catalytic hydrocracking of heavy oils
CA1151579A (fr) * 1981-10-07 1983-08-09 Ramaswami Ranganathan Hydrocraquage d'hydrocarbures lourds avec fort taux de converssion des brais
US4448665A (en) * 1982-12-30 1984-05-15 Exxon Research And Engineering Co. Use of ammonia to reduce the viscosity of bottoms streams produced in hydroconversion processes
DE3326284C2 (de) * 1983-07-21 1985-08-14 Fried. Krupp Gmbh, 4300 Essen Verfahren zur Herstellung flüssiger Kohlenwasserstoffe
DE3442506C2 (de) * 1984-11-22 1987-04-16 Union Rheinische Braunkohlen Kraftstoff AG, 5000 Köln Verfahren zur Aufarbeitung von Kohlenstoff enthaltenden Abfällen
US4623448A (en) * 1985-03-12 1986-11-18 Moreco Energy, Inc. Removing halogenated polyphenyl materials from used oil products
JP3153350B2 (ja) * 1992-07-28 2001-04-09 日本電子株式会社 自動焦点合わせ機能を備えた電子顕微鏡

Also Published As

Publication number Publication date
EP0287796A1 (fr) 1988-10-26
ES2081283T3 (es) 1996-03-01
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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