EP0138215A2 - Procédé d'amélioration de résidus d'hydrogénation du charbon - Google Patents

Procédé d'amélioration de résidus d'hydrogénation du charbon Download PDF

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Publication number
EP0138215A2
EP0138215A2 EP84112308A EP84112308A EP0138215A2 EP 0138215 A2 EP0138215 A2 EP 0138215A2 EP 84112308 A EP84112308 A EP 84112308A EP 84112308 A EP84112308 A EP 84112308A EP 0138215 A2 EP0138215 A2 EP 0138215A2
Authority
EP
European Patent Office
Prior art keywords
hydrogenation
residue
screw machine
distillation
bar
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.)
Ceased
Application number
EP84112308A
Other languages
German (de)
English (en)
Other versions
EP0138215A3 (fr
Inventor
Lothar Ing. Grad. Winckler
Klaus Dr. Dipl.-Chem. Fuhrmann
Ulrich Dr. Dipl.-Ing. Graeser
Peter Dipl.-Ing. Wenning
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.)
Filing date
Publication date
Application filed by Veba Oel Technologie und Automatisierung GmbH filed Critical Veba Oel Technologie und Automatisierung GmbH
Publication of EP0138215A2 publication Critical patent/EP0138215A2/fr
Publication of EP0138215A3 publication Critical patent/EP0138215A3/fr
Ceased 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
    • C10G1/02—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by distillation

Definitions

  • coal is hydrogenated by reaction with hydrogen at temperatures of 250-500 ° C., preferably 350-490 ° C. and pressures of 50-700 bar, preferably 100-350 bar, in particular in the presence of catalysts becomes.
  • the products produced are solid or viscous hydrogenation residues at room temperature.
  • Both hard coal and lignite can be used in the hydrogenation (see W. Krönig, "The catalytic hydrogenation of coal, tars and mineral oils", Springer Verlag, Berlin, Göttingen, Heidelberg 1950).
  • the corresponding technologies were developed and used for technical maturity in the years 1920 to 1945.
  • the hydrogenation technologies according to BERGIUS-PIER and POTT-BROCHE are to be mentioned as basic processes.
  • oils obtained can be used as grinding oils or grinding oil components for the coal.
  • the amounts of oil separated by filtration or spinning contain e.g. T. considerable admixtures of non-evaporable, difficult to hydrogenate, oil-soluble intermediates such.
  • the object of the present invention is to overcome these difficulties. According to the invention, this is done in that the residue of the carbon hydrogenation is subjected to distillation under reduced pressure in a single- or multi-shaft screw machine, the evaporable components are drawn off and the remaining material is introduced into a cooling or granulating device.
  • the hydrogenation residue which constantly increases its viscosity during the distillation, is continuously circulated by screws and thereby passed through the distillation zone of the screw machine, the evaporable constituents being removed from it.
  • Single- or multi-shaft screw machines with gas or steam discharge are known, for. B. from US Pat. Nos. 1,156,096 and 2,615,199. They are used especially in plastics production, and are used there, inter alia, for gas or monomer removal from polymerization mixtures (see M. Herrmann, "Snail machines in process engineering", Springer Verlag, Berlin, Heidelberg, New York 1972). Although the difficulties associated with oil separation have been known since the beginning of the coal hydrogenation on an industrial scale, vacuum screw machines have not been used for processing carbohydrate residues.
  • the processing of hydrogenation residues has different objectives than in the production of plastics:
  • the screw machine is part of the polymerization reactor, whereby the polymerization reaction is terminated by removing the monomers in the vacuum zone, whereas in the case of coal hydrogenation, the enrichment of solids in the hydrogenation residue is effective is.
  • pressures of 0.01 to 0.06 bar preferably 0.02 to 0.1 bar
  • the pressure drops from 0.6, preferably 0.1 bar to 0.01, preferably 0.02 bar over the length of the screw machine from the entry of the hydrogenation sludge to its exit. This measure reduces the risk of disturbances in the distillation process in the screw machine.
  • the distillation of the hydrogenation residue in the screw machine is carried out in particular at temperatures of 200-400 ° C., preferably 250-350 ° C.
  • the temperature rises from 200, preferably 250 ° C. to 400, preferably 350 ° C., under constant pressure or falling over the length of the screw machine. This shortens the time during which the hydrogenation residue assumes high temperatures which favor changes and facilitates further processing of the residue freed from the volatile constituents.
  • Residues up to a final viscosity of approximately 2000 mPas (250 ° C.) can be handled in the distillate removal by the process according to the invention.
  • the gaseous oils withdrawn from the screw machine are expediently used as grating oils or with the other hydrogenating oils, e.g. B. combines the hot separator leaving gaseous hydrogenation products and together with these further treatment, for. B. subjected to a hydrogenation.
  • the rest is introduced from the screw machine directly into a cooling and granulating device.
  • the z. B. can consist of a cooled, circulating belt or a similar device, solidifies the introduced as a viscous mass and can be stored or transported, if necessary after comminution, without the risk of caking, running apart or the like. It is Z. B. usable as fuel or as a feed product of a gasification plant.
  • the present method is suitable for processing all hydrogenation residues which occur in high-pressure coal hydrogenation processes in which coal is mashed with grinding oil and reacted together with hydrogen hydrogen and, if appropriate, in the presence of a catalyst at elevated pressure and elevated temperature, for example by the so-called Bergius-Pier process .
  • a typical gas flame coal of the Ruhr area is mashed with a grinding oil returned from the process and fed together with the hydrogenation hydrogen and with the addition of an iron catalyst at 300 bar and 470 ° C after preheating via line 1 under process pressure hydrogenation reactor 2.
  • the reaction product leaves the reactor 2 via line 3 and is fed to the hot separator 4, in which, under process pressure and at 460 ° C., the products volatile under the prevailing conditions are separated from the solid or liquid reaction products.
  • a positive-conveying pump system 6 which also serves as a metering unit, is used as the conveying element for the feed stream.
  • a vacuum of 0.1 bar is generated in the screw machine 7, which is equipped with a twin screw, via a vacuum line 14.
  • the hydrogenation residue used, which is fed via nozzle 8 to the screw machine 7, contained 0.5 t of oil with a boiling point of 325 ° C. or above, 0.15 t of higher molecular components, which were about 0.1 t as asphaltenes and about 0 , 05 t were determined as pre-asphaltenes, and 0.35 t of inorganic components composed of 0.24 t of ash and 0.11 t of unreacted coal.
  • the ash content was determined to be 32% by weight of SiO 2 , 26% by weight of A1 2 0 3 , 25% by weight of Fe 2 0 3 and 17% by weight of other components.
  • the distillate was separated off at the pressure of 0.1 bar, the hydrogenation residue in the vacuum twin-screw machine 7 being heated from 350 to 450 ° C. during the distillate separation. It evaporated 0.40 t of distillable components of the oil portion, which were withdrawn via connection 9 from the evaporation zone 18 and after cooling, not shown, via line 10 and via condensate container 11 by means of line 13. The uncondensed portions were drawn off via condensate container 11 by means of line 12.
  • the softening point of the residue after passing through the evaporation zone was 180 ° C.
  • the viscosity of the same residue at 250 ° C was determined to be 1500 mPas.
  • the distillable constituents drawn off via line 13 can be returned to the hydrogenation as valuable grinding oil components.
  • the evaporation zone is separated from the discharge zone by a mechanical compression stage 19, which is realized in a known manner by suitable design of the screw and the arrangement of suitable screw elements in this area. This results in a compression of the residue, which contains only 0.1 t of residual oil, in addition to inorganic constituents and higher molecular weight intermediate products, before this residue is fed via connecting piece 14 and line 15 to a cooling belt 16 with subsequent granulating device 17.
  • the screw machine was heated by means of jacket heating of the screw machine using superheated steam.
  • the heating can also be carried out by means of electrically heated heating jaws or by induction heating or, in the case of jacket heating, by flue gas or heat transfer oils.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
EP84112308A 1983-10-15 1984-10-12 Procédé d'amélioration de résidus d'hydrogénation du charbon Ceased EP0138215A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3337624 1983-10-15
DE19833337624 DE3337624A1 (de) 1983-10-15 1983-10-15 Verfahren zur aufarbeitung von rueckstaenden bei der kohlehydrierung

Publications (2)

Publication Number Publication Date
EP0138215A2 true EP0138215A2 (fr) 1985-04-24
EP0138215A3 EP0138215A3 (fr) 1986-12-03

Family

ID=6211991

Family Applications (1)

Application Number Title Priority Date Filing Date
EP84112308A Ceased EP0138215A3 (fr) 1983-10-15 1984-10-12 Procédé d'amélioration de résidus d'hydrogénation du charbon

Country Status (4)

Country Link
EP (1) EP0138215A3 (fr)
CA (1) CA1236418A (fr)
DD (1) DD224609A5 (fr)
DE (1) DE3337624A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2277527A (en) * 1993-03-27 1994-11-02 C G E James Birks Limited Organic waste treatment method and apparatus

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3829986A1 (de) * 1988-09-03 1990-03-15 Enka Ag Verfahren zur erhoehung des mesophasenanteils in pech

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB188686A (en) * 1921-05-17 1922-11-17 Herman Plauson Improvements in the extraction of hydrocarbons from wood
DE737780C (de) * 1940-09-01 1943-07-23 Dr Edwin M F Guignard Kessel zur fraktionierten Destillation von Fluessigkeiten
US2615199A (en) * 1945-05-15 1952-10-28 Welding Engineers Material treating apparatus
DE2327353A1 (de) * 1973-05-29 1975-01-02 Otto & Co Gmbh Dr C Verfahren zur umwandlung fester in fluessige und gasfoermige schwefelarme brennstoffe
DE2407217A1 (de) * 1974-02-15 1975-09-04 Kloeckner Humboldt Deutz Ag Verfahren und vorrichtung zur thermischen behandlung von koernigen feststoffen
DE3227896A1 (de) * 1982-07-26 1984-01-26 Peter 7869 Holzinshaus Voelskow Verfahren zur thermischen behandlung, insbesondere verschwelung, organischer abfaelle und anlage zur ausuebung des verfahrens

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2277527A (en) * 1993-03-27 1994-11-02 C G E James Birks Limited Organic waste treatment method and apparatus

Also Published As

Publication number Publication date
CA1236418A (fr) 1988-05-10
DE3337624A1 (de) 1985-04-25
EP0138215A3 (fr) 1986-12-03
DD224609A5 (de) 1985-07-10

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Inventor name: GRAESER, ULRICH, DR. DIPL.-ING.

Inventor name: FUHRMANN, KLAUS, DR. DIPL.-CHEM.

Inventor name: WENNING, PETER, DIPL.-ING.

Inventor name: WINCKLER, LOTHAR, ING. GRAD.