EP0230543A1 - Procédé de revalorisation d'huile usée - Google Patents

Procédé de revalorisation d'huile usée Download PDF

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Publication number
EP0230543A1
EP0230543A1 EP86116200A EP86116200A EP0230543A1 EP 0230543 A1 EP0230543 A1 EP 0230543A1 EP 86116200 A EP86116200 A EP 86116200A EP 86116200 A EP86116200 A EP 86116200A EP 0230543 A1 EP0230543 A1 EP 0230543A1
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EP
European Patent Office
Prior art keywords
solvent
oil
extraction
waste oil
extraction residue
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
EP86116200A
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German (de)
English (en)
Other versions
EP0230543B1 (fr
Inventor
Rolf Dr. Dipl.-Ing. Wetzel
Hubert Dr. Dipl.-Ing. Coenen
Winfried Dipl.-Ing. Kreuch
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.)
Krupp Koppers GmbH
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Krupp Koppers GmbH
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Publication date
Application filed by Krupp Koppers GmbH filed Critical Krupp Koppers GmbH
Priority to AT86116200T priority Critical patent/ATE41029T1/de
Publication of EP0230543A1 publication Critical patent/EP0230543A1/fr
Application granted granted Critical
Publication of EP0230543B1 publication Critical patent/EP0230543B1/fr
Expired legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
    • C10M175/02—Working-up used lubricants to recover useful products ; Cleaning mineral-oil based

Definitions

  • the invention relates to a process for working up waste oil, in which the previously dewatered waste oil is subjected to extraction under supercritical conditions using a solvent which is gaseous under normal conditions and the extracted components are then separated from the separated supercritical gas phase by reducing the pressure and / or changing the temperature.
  • lubricating oils used technically occur as contaminated waste oils and, as long as they are accessible to a collection, can be used again. This can be done either by incineration for the purpose of energy production or by refining the used oil for the purpose of re-use as a lubricant.
  • the used oil to be processed contains impurities of all kinds, such as metal compounds serving as additives, wear and aging residues and impurities that result from improper storage of the used oil.
  • these contaminants of various types require special measures to protect the environment when burning waste oil and, on the other hand, must be completely separated from the product to be reused when refining the waste oil.
  • the sulfuric acid / bleaching earth process has so far been used to a particularly large extent for refining used oils.
  • the advantages of a simple technique are offset by low yields, insufficient selectivity and larger amounts of problematic waste materials, mainly acid resins and bleaching earth residues.
  • this process does not guarantee the harmless disposal of particularly problematic pollutants such as polychlorinated biphenyls, polychlorinated phenyls, haloalkanes and polycondensed Aromatics.
  • waste oil refining processes are: - the IFP process (replacement of sulfuric acid refining by subcritical propane extraction), - The BERC process (solvent extraction, vacuum fractionation and bleaching earth or H2 aftertreatment), - the CTI process (vacuum thin-film distillation as a purification stage), - The PROP process (application of ammonium phosphates for cleaning and H2 treatment) and - the Recyclon process (separation of the contaminated oil by sodium).
  • IFP process replacement of sulfuric acid refining by subcritical propane extraction
  • the BERC process solvent extraction, vacuum fractionation and bleaching earth or H2 aftertreatment
  • CTI process vacuum thin-film distillation as a purification stage
  • PROP process application of ammonium phosphates for cleaning and H2 treatment
  • Recyclon process separation of the contaminated oil by sodium
  • the CTI process with a thin-film evaporator as a physical cleaning stage was used on an industrial scale.
  • the problems of thin-layer evaporation consist in fouling the heat exchanger surfaces and in the comparatively low selectivity of the process.
  • the invention is therefore based on the object of further developing the method for processing waste oil using supercritical extraction in such a way that the above-described disposal problem is solved in a surprising manner, so that the processing of the waste oil without the occurrence of residues or unacceptably polluting the environment By-products can be carried out.
  • the method according to the invention basically provides two options for the disposal of the resulting solvent-free extraction residue. If conditions permit, efforts will be made to dispose of the extraction residue by storage in a landfill for cost reasons. However, if this is not possible, the extraction residue will be disposed of by thermal treatment (gasification).
  • the waste oil to be processed is fed from the collecting container 1 via line 2 to the filter system 3, in which the solid particles are separated from the waste oil by filtration and are withdrawn via line 4.
  • the waste oil freed from the solid particles reaches the distillation column 7 via line 5 and the pump 6.
  • the waste oil is subjected to a distillation in the temperature range between 12 ° C. and 25 ° C. under atmospheric pressure.
  • the gas oil-water mixture escaping overhead from the distillation column 7 is introduced via line 8 into the separating tank 9, in which the water is separated from the gas oil (so-called gas oil I) by phase separation is separated.
  • the gas oil is withdrawn through line 10 and the water through line 11 from the separating tank 9.
  • the pre-distilled and dewatered waste oil withdrawn via line 12 from the distillation column 7 is introduced into the central part of the extraction column 13, which works at a pressure between 5o and 15o bar and a temperature between 2o ° C and 8o ° C.
  • the pump 14 brings the waste oil to the required operating pressure of the extraction column 13 and the heat exchanger 15 ensures that the required operating temperature of the waste oil is reached.
  • the waste oil can also be fed into the extraction column 13 in its upper or lower part.
  • the required solvent is introduced via line 16 into the lower part of the extraction column 13.
  • the solvent absorbs the components of the waste oil that are soluble under the specified operating conditions, while the insoluble components collect together with the impurities in the bottom of the extraction column 13 and are withdrawn from there via line 17 under level control.
  • the valve 18 serves to regulate the extraction of the extraction residue from the extraction column 13.
  • the necessary expansion of the extraction residue to a pressure of 1 to 0.1 bar takes place in the expansion tank 19.
  • the gaseous solvent released in this process is removed via line 20.
  • the expansion tank 19 can be heated and provided with an agitator.
  • the upper part of the extraction column 13 acts as an amplifier section.
  • the top product obtained there is drawn off via line 21 and enters the steam-heated heat exchanger 22, in which the required reflux is generated by a slight increase in temperature, since the solubility of the oil in the supercritical solvent decreases as the temperature increases.
  • the downstream separator 23 the condensed oil is separated off and returned to the extraction column 13 by the pump 24 via line 25, where it is added as reflux to the top of the column.
  • the loaded solvent passes from the separator 23 via the line 26 into the high-pressure separator 27, in which, in the present case, the oil phase is completely separated from the solvent.
  • the separated oil phase which is the extract
  • the low-pressure separator 29 is withdrawn from the lower part of the high-pressure separator 27 in a level-controlled manner and reaches the low-pressure separator 29 via line 28, in which the solvent residues still present in the oil phase are separated off.
  • the amount of the extract drawn off via line 28 is regulated by valve 3o.
  • the solvent-free product oil is withdrawn via line 31 from the low-pressure separator 29 and passes via line 31 into the collecting container 32.
  • the product oil is pressed into the hydrogenation reactor 36 via the pump 34 located in line 33 and the heat exchanger 35 which is the catalytic hydrogenation of the product oil in the presence of commercially available hydrogenation catalysts which contain, for example, nickel as the active component, he follows.
  • the hydrogen required for this is introduced into the hydrogenation reactor 36 via line 37.
  • the halogen and sulfur compounds contained in it are converted into hydrogen or hydrogen sulfide.
  • These products are withdrawn in gaseous form from the hydrogenation reactor 36 via line 38.
  • the hydrogenated product oil in the meantime passes via line 39 into the addition container 4o, into which bleaching earth can be introduced via line 41, which is mixed in the addition container 4o with stirring with the hydrogenated product oil.
  • the bleaching earth / oil mixture is then introduced via the pump 42 and the line 43 into the vacuum distillation column 44, in which it is distilled under a vacuum of from o, oo2 to o, 1 bar and is thus broken down into different fractions.
  • the hydrogenated product oil passes directly into the vacuum distillation column 44 via line 39.
  • Gas oil II is withdrawn via line 45 and spindle oil is removed via line 46.
  • the distillation residue obtained in the vacuum distillation column 44 is conveyed by means of the pump 48 in line 47 into the filter system 49, in which the bleaching earth is separated off by filtration. This oiled bleaching earth passes through line 51 into the gasifier 52, while the base oil obtained during the filtration is drawn off from the filter system 49 via line 50.
  • the following products are also introduced into the gasifier 52: the extraction residue from the expansion tank 19 via the line 53 and the pump 54, the gas oil I from the Separating tank 9 via line 10 and the sewage sludge from biological wastewater treatment 55 via line 56.
  • the gasifier 52 can be an entrained flow gasifier which works according to the known Koppers-Totzek method. Oxygen and / or air and possibly small amounts of water vapor serve as the gasification medium. The gasification can be carried out under normal or increased pressure. If liquids or suspensions are to be gasified, the gasifier is equipped with so-called atomizing burners. The burners can also be preceded by heat exchangers in which the product to be gasified is brought to the temperature required for setting the required viscosity.
  • the products introduced into the gasifier 52 are gasified in a flame reaction at temperatures between 13oo ° C and 2ooo ° C.
  • the additional fuel which may be required for this purpose passes through line 57 and the required air or oxygen via line 58 into the gasifier 52.
  • the gas which is essentially composed of the components CO, H2, CO2, H2O and N2 is fed via line 59 withdrawn from the carburetor 52 and passes through the waste heat boiler 6o into the pressurized water scrubber 61.
  • the gas stream from the line 38 is also introduced into this, so that both gas streams pass through the subsequent gas treatment together.
  • This consists of the pressurized water wash 61 and the pressurized wash 62, the individual stages being connected to one another via the lines 63 and 64.
  • This gas treatment removes both halogen and hydrogen sulfide as well as the metal compounds originating from the oil additives from the gas. Since the gas in the waste heat boiler 6o has already been pre-cooled to the required extent, the gas drawn off after passing through the two washing stages via line 65 can be used without problems as heating gas.
  • the gasification residue (slag) obtained in the gasification is drawn off in the molten state via line 66 from the gasifier and granulated and cooled in a water bath (not shown).
  • the solvent escaping overhead from the high-pressure separator 27 is drawn off via line 67 and returns via the heat exchanger 68 to line 16, via which the solvent is reintroduced into the extraction column 13. Since the solvent circuit is almost isobaric, only a slight increase in pressure has to be brought about by the circuit compressor 69.
  • the heat exchangers 68 and 70 serve the required temperature setting of the solvent.
  • the solvent escaping from the low-pressure separator 29 is drawn off via the line 71 and, after having been compressed to condensation pressure in the compressor 72, reaches the condenser 73, in which it is liquefied.
  • the heat exchanger 74 in turn serves the required temperature setting.
  • Line 2o opens into line 71 in front of heat exchanger 74, via which line the solvent released in expansion tank 19 is drawn off.
  • the liquefied solvent is collected in the template 75 and fed from there through the compressor 76 via line 77 into line 16, if necessary.
  • the water separated in the separating container 9 passes through line 11 into the biological wastewater treatment 55, from which the cleaned wastewater is introduced via line 78 into the receiving water.
  • the sewage sludge resulting from the wastewater treatment is, as already mentioned, fed to the gasifier 52 via line 56.
  • the dry oil emerging from the distillation column 7 was cooled to 43 ° C. via the heat exchanger 15, compressed to 100 bar with the pump 14 and then fed to the extraction column 13 at half the height. At the foot of the extraction column 13, ethane was fed in as a solvent at 43 ° C. and 100 bar.
  • the soluble constituents of the dry oil were taken up by the solvent by countercurrent extraction.
  • the loaded solvent phase was fed to the heat exchanger 22 (dephlegmator) and heated to 48 ° C. This resulted in a partial separation of the low volatility hydrocarbons (denatured additives), which flowed against the rising loaded solvent phase and caused a stripping effect, which achieved an additional separation effect.
  • the dry oil applied could be separated into an extraction residue of 14 kg / h and a value fraction of 126 kg / h.
  • the extraction residue was drawn off at the foot of the extraction column 13, let down to 1 bar and heated to 150 ° C.
  • the solvent released was recompressed and fed to the main solvent stream.
  • the cleaned loaded solvent phase (extract) was freed from the dissolved products after the heat exchanger 22 in the downstream high-pressure separator 27 by heating to 150 ° C. at 100 bar.
  • the separated product in an amount of 126 kg / h was drawn off at the bottom of the high-pressure separator 27 and expanded to 1 bar in the low-pressure separator 29 in order to separate off the solvent still dissolved in it.
  • the solvent released was recompressed and combined with the main solvent stream.
  • the separated product was subjected to hydrogenation in the hydrogenation reactor 36 to break down the halogenated hydrocarbons present in it and then separated into the products base oil, spindle oil and gas oil II in the vacuum distillation column 44. 2.8 kg / h of bleaching earth were added to the product given to the vacuum distillation.
  • the oily bleaching earth was filtered off from the bottom product of the vacuum distillation in the filter system 49. 74 kg / h base oil, 35 kg / h spindle oil and 14 kg / h gas oil II as well as 5.6 kg / h oiled bleaching earth were obtained.
  • the extraction residue preheated to 150 ° C. was compressed to the required admission pressure of the gasifier 52.
  • the gas oil I was mixed with the oil-laden bleaching earth and the small amount of sewage sludge obtained in the biological wastewater treatment 55 and the resulting mixture was also compressed to the required admission pressure of the gasifier 52 and fed to the gasifier 52 together with the extraction residue at approx. 150 ° C.
  • This mixture was under in the carburetor 52 Addition of o, 95 kg oxygen per kg mixture as an oxidizing agent in a flame reaction at temperatures above 15oo ° C gasified.
  • the product of gasification was CO and H2 in a ratio of 2.1: 1 as well as small amounts of CO2 and water vapor as well as traces of H2S and HCl.
  • the metal contents of the residue were oxidized and removed from the carburetor as ash or fly dust.
  • the hot raw gas which was still loaded with small amounts of flying dust, was subjected to the gas treatment described above, whereby heating gas, waste heat steam and saline solution were obtained.
  • it was mixed with the raw gas from the gasification before the gas treatment.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Lubricants (AREA)
  • Processing Of Solid Wastes (AREA)
  • Fats And Perfumes (AREA)
  • Treatment Of Sludge (AREA)
EP86116200A 1986-01-29 1986-11-21 Procédé de revalorisation d'huile usée Expired EP0230543B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT86116200T ATE41029T1 (de) 1986-01-29 1986-11-21 Verfahren zur aufarbeitung von altoel.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3602586 1986-01-29
DE19863602586 DE3602586A1 (de) 1986-01-29 1986-01-29 Verfahren zur aufarbeitung von altoel

Publications (2)

Publication Number Publication Date
EP0230543A1 true EP0230543A1 (fr) 1987-08-05
EP0230543B1 EP0230543B1 (fr) 1989-03-01

Family

ID=6292841

Family Applications (1)

Application Number Title Priority Date Filing Date
EP86116200A Expired EP0230543B1 (fr) 1986-01-29 1986-11-21 Procédé de revalorisation d'huile usée

Country Status (6)

Country Link
US (1) US4797198A (fr)
EP (1) EP0230543B1 (fr)
JP (1) JPS62184097A (fr)
AT (1) ATE41029T1 (fr)
DE (2) DE3602586A1 (fr)
ES (1) ES2006695B3 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU638922B1 (fr) * 1992-10-01 1993-07-08

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3839799A1 (de) * 1988-11-25 1990-07-05 Rwe Entsorgung Ag Verfahren zur aufarbeitung kontaminierter oele
US5143597A (en) * 1991-01-10 1992-09-01 Mobil Oil Corporation Process of used lubricant oil recycling
US5316743A (en) * 1992-09-28 1994-05-31 Leblanc Ralph W Diesel fuel cracking unit
FR2725725B1 (fr) * 1994-10-17 1996-12-13 Inst Francais Du Petrole Procede et installation pour la purification des huiles usagees
US6066350A (en) 1997-02-07 2000-05-23 Cargill Incorporated Method and arrangement for processing cocoa mass
US7045038B1 (en) * 1999-12-21 2006-05-16 Industrial Microwave Technologies, Inc. Process for treating waste oil
EP1279722A1 (fr) * 2001-07-18 2003-01-29 Minitec Engineering GmbH Procédé de purification d'huiles et d'élimination des dépôts solides,dans des systèmes contenant de l'huile,des échangeurs de chaleur tubulaires,des transformateurs,des réservoirs de stockage ou similaires
US20040071848A1 (en) * 2002-10-15 2004-04-15 Cargill Inc. Process for producing cocoa butter and cocoa powder by liquefied gas extraction
US20040071847A1 (en) * 2002-10-15 2004-04-15 Cargill, Inc. Producing cocoa powders with different cocoa butter contents by liquefied gas extraction on substantially the same production line
US7201934B2 (en) * 2002-10-15 2007-04-10 Cargill, Incorporated Dispersible cocoa products
US8088276B2 (en) * 2008-08-08 2012-01-03 CleanOil Limited Oil re-refining system and method
WO2020160662A1 (fr) * 2019-02-05 2020-08-13 Gen Iii Oil Corporation Procédé et système de reraffinage et de valorisation d'huile usagée

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2030609A1 (de) * 1969-09-09 1971-03-18 Petrolchemisches Kombinat Verfahren zur Aufarbeitung von ge brauchten Schmierölen
US3919076A (en) * 1974-07-18 1975-11-11 Pilot Res & Dev Co Re-refining used automotive lubricating oil

Family Cites Families (13)

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US3074882A (en) * 1959-02-02 1963-01-22 Texaco Inc Petroleum treating process involving solvent deasphalting and propane fractionation
US3507777A (en) * 1968-01-25 1970-04-21 Exxon Research Engineering Co Cracking process
US3594308A (en) * 1970-06-22 1971-07-20 Universal Oil Prod Co Petroleum crude oil conversion process
US3864242A (en) * 1973-12-13 1975-02-04 Imamura Seisakusho Kk Treating muddy-like waste oily material
US4021333A (en) * 1975-08-27 1977-05-03 The Lubrizol Corporation Method of rerefining oil by distillation and extraction
IT1091961B (it) * 1978-01-12 1985-07-06 Snam Progetti Procedimento per la rigenerazione degli oli esausti
DE2850540C2 (de) * 1978-11-22 1982-12-23 Fried. Krupp Gmbh, 4300 Essen Verfahren zur Aufbereitung von Altöl
CS209612B1 (en) * 1979-11-10 1981-12-31 Alexander Tkac Method of treating the spent motor oils
US4363717A (en) * 1981-01-15 1982-12-14 Mobil Oil Corporation Conversion of heavy hydrocarbon oils
IT1137280B (it) * 1981-07-07 1986-09-03 Assoreni E Snamprogetti Spa Procedimento per recupero di oli esausti
US4482453A (en) * 1982-08-17 1984-11-13 Phillips Petroleum Company Supercritical extraction process
DE3321356A1 (de) * 1983-06-14 1984-12-20 Drägerwerk AG, 2400 Lübeck Gasdosimeter in einer halterung, ein diffusionspruefroehrchen enthaltend
US4431523A (en) * 1983-06-24 1984-02-14 Phillips Petroleum Company Upgrading fuel fractions in a re-refined oil process

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2030609A1 (de) * 1969-09-09 1971-03-18 Petrolchemisches Kombinat Verfahren zur Aufarbeitung von ge brauchten Schmierölen
US3919076A (en) * 1974-07-18 1975-11-11 Pilot Res & Dev Co Re-refining used automotive lubricating oil

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU638922B1 (fr) * 1992-10-01 1993-07-08

Also Published As

Publication number Publication date
ATE41029T1 (de) 1989-03-15
JPS62184097A (ja) 1987-08-12
EP0230543B1 (fr) 1989-03-01
US4797198A (en) 1989-01-10
ES2006695B3 (es) 1989-10-16
DE3602586A1 (de) 1987-07-30
DE3662205D1 (en) 1989-04-06

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