EP0249748B1 - Verfahren zur hydrierenden Spaltung von Kohlenstoff enthaltenden Abfällen in der Wirbelschicht - Google Patents

Verfahren zur hydrierenden Spaltung von Kohlenstoff enthaltenden Abfällen in der Wirbelschicht Download PDF

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Publication number
EP0249748B1
EP0249748B1 EP87107059A EP87107059A EP0249748B1 EP 0249748 B1 EP0249748 B1 EP 0249748B1 EP 87107059 A EP87107059 A EP 87107059A EP 87107059 A EP87107059 A EP 87107059A EP 0249748 B1 EP0249748 B1 EP 0249748B1
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EP
European Patent Office
Prior art keywords
waste
hydrogen
process according
wastes
hydrogenating
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.)
Expired - Lifetime
Application number
EP87107059A
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German (de)
English (en)
French (fr)
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EP0249748A1 (de
Inventor
Joachim Dr. Korff
Hans Dr. Gierlich
Wilfried Dr. Dolkemeyer
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.)
RWE Entsorgung AG
Original Assignee
Rheinbraun AG
Rheinische Braunkohlenwerke AG
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Application filed by Rheinbraun AG, Rheinische Braunkohlenwerke AG filed Critical Rheinbraun AG
Priority to AT87107059T priority Critical patent/ATE56220T1/de
Publication of EP0249748A1 publication Critical patent/EP0249748A1/de
Application granted granted Critical
Publication of EP0249748B1 publication Critical patent/EP0249748B1/de
Anticipated expiration legal-status Critical
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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

Definitions

  • the present invention relates to a process for the hydrogenative cleavage of carbon-containing wastes in the fluidized bed.
  • Waste has been used in landfills for decades, e.g. stored in abandoned gravel pits, mine pits and elsewhere. For a long time, the chemical structure of the waste and its long-term effects on soil and groundwater have not been taken into account. More recently, certain waste has been stored in so-called special landfills.
  • Pyrolysis is now also being operated on a technical scale (see, for example, "United Economic Services GmbH", 4 Oct. 1985, pg).
  • pyrolysis has the disadvantages of the predominant formation of gaseous products and a heavily contaminated coke residue.
  • EP-A 0 182 309 discloses the hydrogenative cleavage of waste containing carbon in a reactor with a downstream hot separator, that is to say under so-called bottom phase conditions.
  • the feed mixture in pumpable or extrudable form is fed into a hydrogenation reactor from bottom to top, together with hydrogen, which is also generally pumped from bottom to top into the reactor.
  • the vaporizable oil fraction is separated from the residue remaining in the sump.
  • NL-A 8 402 641 (EP-A 175 406) describes the hydrogenative cleavage of polyhalogenated compounds at temperatures of 800 ° -1200 ° C., very short residence times of 1-10 s and normal pressure.
  • the present invention discloses a surprising solution to this problem, which is considerably cheaper than in the prior art, particularly with regard to the recovery of very high proportions of valuable products, for the recovery of hydrocarbons from carbon-containing wastes by hydrogenative cleavage of the carbon-containing wastes with hydrogen and / or Hydrogen-containing gases and / or hydrogen-donating compounds, characterized in that the hydrogenating cleavage takes place in the fluidized bed at 250-900 ° C and 5-280 bar.
  • This process makes it possible to process waste from which larger inorganic constituents of glass, metals, stone materials and the like are largely removed without further sorting to valuable hydrocarbons, i.e. to C, -C 4 hydrocarbons, to hydrocarbons boiling in the gasoline sector and to agents - and heavy oils that can be used as diesel oil and for heating purposes. It is also of particular advantage that the products used need only be comminuted a little, that the products are practically olefin-free and that hetero elements are obtained as hydrogen compounds which can be easily worked up according to the prior art.
  • Pre-sorted materials can also be processed in accordance with this method, in particular in such a way that, for example, mixtures of carbon-containing waste containing synthetic waste in household waste jumps, such as plastics or plastic mixtures, rubber, tires, textile waste and the like, are at least roughly separated from the vegetable or biomass portion and then subjected to the hydrating treatment, possibly together with industrial waste, such as paint and paint residues and organic Chemicals, industrial production waste, organic synthetic shredder waste from the automotive industry, cable waste, used tires, sewage sludge or with used oils and the like. The like.
  • other wastes such as paper, food residues, agricultural and forestry wastes, wood, plants and the like can be largely separated off, but also to a certain extent remain in the synthetic portion.
  • the synthetic individual components can also be processed very well into valuable liquid products under the conditions according to the invention.
  • production-specific or waste-generator-specific waste can also be used, at least temporarily, separately from other types of waste.
  • shredder waste usually consists of plastic mixtures, cable waste from mixtures of different components, textile waste from mixtures.
  • waste producer or production-specific waste can be used at least temporarily, for example until a supply of such waste has been used up.
  • non-waste producer or production-specific waste can also be implemented, i.e. mixtures of several types of waste or e.g. Mixtures of synthetic-organic waste as they occur in waste separation plants.
  • coal components such as, for example, coal oil residues, coal oils, pyrolysis oils, petroleum, petroleum residues, other petroleum components, oil shale, oil shale components, oil sands, bitumen and the like or the like Mixtures of these materials. It is generally known that in the case of the simultaneous hydrolytic cleavage of these additives, numerous catalysts are suitable.
  • the carbon-containing wastes to be reacted with hydrogen and / or hydrogen-containing gases and / or hydrogen-releasing compounds are reacted with these gases in a fluidized bed, if appropriate in the presence of biomass or other vegetable or cellulose-containing materials, with the aid of the gases mentioned which Fluidized bed is at least partially generated or maintained.
  • the gases can additionally contain other components, such as, for example, N 2 , CO, C0 2 , CH 4 or water vapor. However, the total amount of gases contains 25% by volume of hydrogen.
  • Both state-of-the-art reactors and further developed fluidized-bed reactors can be used as fluidized-bed reactors.
  • the solid, carbon-containing wastes used can be comminuted to different material sizes or can also be used without comminution.
  • a solid carrier material can be used both in a straight pass and at least partially recycled.
  • Such materials can be, for example, inert materials, such as sand, gravel, corundum, ceramics, clay, coke or the like, and these materials can also serve as heat carriers.
  • it can also be catalytically active solid materials such as, for example, Fe, Mo, Ni, Co, W and other hydrogenation-active metals and / or catalysts containing their compounds, which may consist of individual or at least two of these components and the metals and / or whose compounds can be applied to carriers, for example to aluminum oxide, silicon dioxide, aluminum silicates, zeolites, the solid additional materials mentioned above and other carriers known to the person skilled in the art or from carrier mixtures. However, they can also be used without a carrier. Certain zeolites as such are also suitable.
  • Suitable catalysts can be so-called disposable catalysts, such as hearth furnace coke, Winkler gasification dusts, dusts and ashes, which are obtained in the hydrogenating gasification of coal to methane (HKV dusts), but also mixtures containing iron oxides and other iron compounds, such as red mud, Bavarian mass, Lux mass, dusts from the iron industry and others, these materials also being able to be doped with hydrogenation-active metals and / or metal compounds, in particular with heavy metal salts, such as iron salts or salts of chromium, zinc, molybdenum, tungsten, Manganese, nickel, cobalt, also with alkali, alkaline earth, among others, as well as with mixtures of this compound. fertilize.
  • disposable catalysts such as hearth furnace coke, Winkler gasification dusts, dusts and ashes, which are obtained in the hydrogenating gasification of coal to methane (HKV dusts), but also mixtures containing iron oxides and other iron compounds, such as red
  • At least some of the catalysts can be pretreated sulfiding. It goes without saying that all of the support materials and catalysts mentioned can be used both individually and in mixtures.
  • the fluidized bed area can consist of liquid waste or molten solid waste, the additives mentioned, e.g. Residual oils, coal, etc. may also be included, and solid finely divided catalysts or inert solid materials or both are kept in a swirling motion within the liquid by the supplied gas.
  • the additives mentioned e.g. Residual oils, coal, etc. may also be included, and solid finely divided catalysts or inert solid materials or both are kept in a swirling motion within the liquid by the supplied gas.
  • the fluidized bed process can also be carried out without the presence of liquid or in the presence of only a little liquid product.
  • the conditions of the hydrogenating reaction according to the invention can be varied within wide limits depending on the starting products.
  • the temperature is 250 to 900 ° C., preferably 350 to 800 ° C. and particularly preferably 400 to 600 ° C.
  • the pressure is 5 to 280 bar and preferably 8 to 240 bar.
  • the ratio of hydrogen to the feed product is determined in particular by the amount of gas required in the case of a certain piece or particle size or amount of the solid and / or liquid feed product which is necessary to maintain the fluidized bed.
  • the gas velocity can be 0.05 to 1.5 m / s, preferably 0.2 to 1 m / s, but can also be up to 30 m / s in the case of so-called fast.riser fluidized beds to reach.
  • the maintenance of the fluidized bed and the flow rate of the liquids used are also determined by adding other gases and adding water vapor.
  • All hydrogen qualities can be used as hydrogenation gas, also with admixtures such as CO, C0 2 , H 2 S, methane, ethane, water vapor, etc.
  • Hydrogen qualities such as those which arise in the gasification reactions of carbon-containing materials with water vapor, are very suitable.
  • Such materials can be residues from the processing of mineral oils or coal, wood, peat or residues from the coal processing, for example hydrogenation.
  • Biomass or the vegetable parts separated from household waste are also suitable.
  • the feed product can be mixed with coal and / or coal components and / or petroleum residues and / or petroleum and others. be hydrogenated.
  • Suitable solvents are e.g. Tetralin, anthracene oil, isopropanol, oils containing cresol, decalin, naphthalene, tetrahydrofuran, dioxane, but also, for example, petroleum-derived hydrocarbons and oils and oxygen-containing hydrocarbons and oils.
  • water or steam can also be added.
  • waste mixtures can also be processed in a hydrogenating manner in such a way that mixtures of vegetable and synthetic waste, optionally with the addition of biomass, are implemented in various stages under conditions in which, on the one hand, the hydrolytic and / or hydrogenating conversion of vegetable or Paper and biomass and on the other hand the hydrogenation of the synthetic organic waste takes place.
  • a hydrogenating treatment can optionally be carried out in the presence of hydrogenation catalysts and a pressure of up to 150 bar, preferably 25-60 bar, preferably two se in the presence of water and other protic solvents such as alcohols.
  • oils obtained predominantly from the vegetable portion can then be separated off by solvent extraction, after which the portion which is not hydrolyzed can be hydrolyzed in the fluidized bed in the second stage under the conditions already described.
  • the stepwise processing can also be carried out in such a way that vegetable parts or paper parts or biomass are hydrolytically split in the first step, for example in the presence of alkalis or acids, this reaction possibly taking place in the presence of CO and preferably in the presence of water and / or other protic solvents such as alcohols and in the second stage the synthetic or predominantly synthetic portion in the fluidized bed is reacted in a hydrogenating manner.
  • the waste and / or the biomass can be separated beforehand into a vegetable portion and a synthetic portion and processed separately under the conditions described.
  • the waste to be hydrogenated and / or the biomass can also be used in the presence of hydrogen or gases containing it and / or in the presence of hydrogen-transferring compounds, in particular so-called hydrogen donor solvents, but also in the presence of inert gases, that is to say thermally in mixing devices. pretreat in particular in extruders and mixing / kneading devices.
  • Numerous other mixing devices such as, for example, kneading disc screw presses, kneaders, hollow screw heat exchangers, screw kneaders, kneading extruders, stirring apparatuses, continuous mixers, reaction mixers, kneaders, grinding devices or mills such as bead, hammer or vibrating mills are suitable for the pretreatment according to the invention .
  • the method according to the invention makes it possible to process even little or no pre-separated waste mixtures.
  • inorganic materials such as stones, metals, glass and the like beforehand, at least rough materials.
  • Pre-separation into, for example, predominantly vegetable or cellulose-containing and predominantly synthetic materials can also take place, the vegetable part being able to be processed separately, for example in a fermentation.
  • Solvents containing polychlorobiphenyls, PVC, fluoropolymers or halogens may be mentioned here by way of example.
  • the waste materials can also be used for petroleum, petroleum components and derived products, coal, coal components and derived products, asphalts, bitumen, oils from pyrolysis e.g. from coking or waste pyrolysis, oil sand products, oil shale products, heavy residual oils and the like are added and processed together.
  • metal-containing wastes can be processed in a particularly advantageous manner, since the metals are obtained in the form of ashes after the hydrogenation and can then be subjected to metal processing.
  • the reaction zone can consist of one or more reactors connected in series or in parallel.
  • the liquid hydrocarbons obtained can be processed further in accordance with the prior art, for example by means of further hydrogenating cracking stages or refining stages and separation by distillation.
  • the uncondensed gases are scrubbed of H 2 S, NH 3 , HCl, and possibly also CO and C0 2 .
  • the hydrogen in the resulting gas can be returned to the hydrogenation reactor (s) as hydrogenation gas.
  • the liquid products can be fed to a refining stage which generally works in a hydrogenating manner. Small amounts of compounds containing heteroatoms which are still present can be worked up completely by hydrogenation, so that the products are then practically free of sulfur, nitrogen and halogen. Higher-boiling fractions can be fed to at least one cracking plant, in particular a hydrocracking plant. If necessary, certain portions of the processing can be returned to the waste hydrogenation or before the waste hydrogenation.
  • the process according to the invention can also be combined with other waste hydrogenation processes, such as, for example, a bottom phase hydrogenation.
  • a waste mixture of the green bin consisting of foils, hard plastics, textile and paper parts, which had been obtained after the previous separation of the reusable components such as metals, glass and paper, was at 470 ° C and 60 bar in the fluidized bed (quartz sand) implemented with hydrogen.
  • a gas phase (9% by weight), 75% liquid products in the boiling range up to 390 ° C. and 16% residue (inert materials, carbon black and high boilers) were obtained as products.
  • the gas phase contained 2% CO and C0 2 .
  • Example 1 was repeated, calcium oxide being added to the feed. An HCI-free gas phase was obtained with the product composition unchanged within the scope of the analysis accuracy. The HCI released from the PVC components was thus almost completely bound.
  • a mixture of synthetic waste which consisted of daily samples from several waste separation plants, was reacted with hydrogen at 480 ° C. and 100 bar into the fluidized bed (cobalt / molybdenum catalyst on A1 2 0 3 ) without further purification.
  • the hydrogenation was practically quantitative, but a higher gas content was obtained compared to Example 1, which is due to the higher paper and biomass content.
  • a product was obtained which consisted of 17% gas phase, 70% liquid product in the boiling range up to 390 ° C. and 13% residue (carbon black, inert materials).
  • a product was obtained which contained 64% hydrocarbons in the boiling range up to 390 ° C.
  • the gas phase which was 12% of the total product, contained 3.5% CO / CO 2 .
  • the residue consisted essentially of inert materials such as metals, fillers, etc. and carbon black.
  • Synthetic-organic waste components including PVC from a daily sample from a waste separation plant were brought into the fluidized bed reactor together with residues from mineral oil processing.
  • the plastic content in use was 60% by weight.
  • the fluidized bed consisted of aluminum silicate impregnated with iron compounds.
  • reaction gas 5% by weight contained only traces of CO and CO 2 and the amounts of HCl corresponding to the PVC used.
  • a mixture of PVC-containing plastic waste from a waste sorting plant was introduced into the fluidized bed reactor together with chlorine-contaminated oils and organic chemical residues which contained 1% by weight of chlorine.
  • the plastic content was 60% by weight.
  • aluminum silicates containing nickel / molybdenum this mixture was reacted with hydrogen at 480 ° C and 50 bar.
  • a mixture of tire waste, paint residue and wood waste was implemented without a carrier at 490 ° C and 120 bar. 54 wt.% To 390 ° C. boiling oils, 25 wt.% Gases including small amounts of CO and CO 2 and 21 wt.% Solids (metal residues, soot, pigment components) were obtained as the product.
  • a mixture of shredded waste cables, old tires, wood and coal particles was in the presence implemented a furnace coke doped with FeS0 4 as a catalyst at 460 ° C and 150 bar.
  • the product obtained was 34% by weight of oils which boiled at up to 390 ° C., 30% by weight of gases and 36% by weight of solids (in particular cable metal residues and carbon black).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Processing Of Solid Wastes (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Catalysts (AREA)
  • Treating Waste Gases (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
EP87107059A 1986-05-17 1987-05-15 Verfahren zur hydrierenden Spaltung von Kohlenstoff enthaltenden Abfällen in der Wirbelschicht Expired - Lifetime EP0249748B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87107059T ATE56220T1 (de) 1986-05-17 1987-05-15 Verfahren zur hydrierenden spaltung von kohlenstoff enthaltenden abfaellen in der wirbelschicht.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19863616785 DE3616785A1 (de) 1986-05-17 1986-05-17 Verfahren zur aufarbeitung von kohlenstoff enthaltenden abfaellen und biomassen
DE3616785 1986-05-17

Publications (2)

Publication Number Publication Date
EP0249748A1 EP0249748A1 (de) 1987-12-23
EP0249748B1 true EP0249748B1 (de) 1990-09-05

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EP87107059A Expired - Lifetime EP0249748B1 (de) 1986-05-17 1987-05-15 Verfahren zur hydrierenden Spaltung von Kohlenstoff enthaltenden Abfällen in der Wirbelschicht

Country Status (6)

Country Link
EP (1) EP0249748B1 (es)
AT (1) ATE56220T1 (es)
DD (1) DD260712A5 (es)
DE (2) DE3616785A1 (es)
ES (1) ES2000629B3 (es)
GR (2) GR880300007T1 (es)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3719824C1 (de) * 1987-06-13 1989-03-09 Felten & Guilleaume Energie Verfahren und Vorrichtung zur gezielten Zerlegung (Cracken) von Halogenkohlenwasserstoffen mit anschliessender umweltfreundlicher Aufbereitung der gecrackten Stoffe
DE3912807A1 (de) * 1989-04-19 1990-11-08 Gfk Kohleverfluessigung Gmbh Katalysator bzw. additiv zur hydrierenden behandlung von schweren erdoelen bzw. schweren erdoelfraktionen sowie verfahren zur gewinnung des katalysators
US5435983A (en) * 1990-07-02 1995-07-25 University Of Hawaii Process for charcoal production from woody and herbaceous plant material
BE1010022A3 (fr) 1996-02-29 1997-11-04 Solvay Procede de recyclage de dechets plastiques.
US6653410B1 (en) 1998-11-04 2003-11-25 Asahi Kasei Kabushiki Kaisha Method for treating resin composition
DE102005040490A1 (de) * 2005-07-25 2007-02-08 Demir, Yaver Vorrichtung und Verfahren für eine Biokraftstoff Raffinerie: Direkte thermochemische Umwandlung von organischen Substanzen in flüssige Brennstoffe

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL8402641A (nl) * 1984-08-30 1986-03-17 Univ Leiden Werkwijze voor het vernietigen van organische afvalstoffen door thermische omzetting.

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3540995A (en) * 1968-11-14 1970-11-17 Us Interior H-coal process:slurry oil system
US3704108A (en) * 1970-09-25 1972-11-28 Hydrocarbon Research Inc Hydroconversion of waste natural and synthetic rubbers
US3714038A (en) * 1970-12-18 1973-01-30 Black Clawson Co Process and product for converting organic materials by pyrolysis or hydrogenation
JPS5729246B2 (es) * 1973-05-09 1982-06-22
GB2106128A (en) * 1981-07-18 1983-04-07 Inst Gas Technology Production of synthetic liquid and gaseous hydrocarbon fuels from peat
DE3442506C2 (de) * 1984-11-22 1987-04-16 Union Rheinische Braunkohlen Kraftstoff AG, 5000 Köln Verfahren zur Aufarbeitung von Kohlenstoff enthaltenden Abfällen

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL8402641A (nl) * 1984-08-30 1986-03-17 Univ Leiden Werkwijze voor het vernietigen van organische afvalstoffen door thermische omzetting.

Also Published As

Publication number Publication date
EP0249748A1 (de) 1987-12-23
DE3764719D1 (de) 1990-10-11
GR3000897T3 (en) 1991-11-15
ES2000629A4 (es) 1988-03-16
DD260712A5 (de) 1988-10-05
DE3616785A1 (de) 1987-11-19
ATE56220T1 (de) 1990-09-15
ES2000629B3 (es) 1990-12-01
GR880300007T1 (en) 1989-06-22

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