EP0708174B1 - Verfahren und Anlage zur Reinigung von Altölen - Google Patents

Verfahren und Anlage zur Reinigung von Altölen Download PDF

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Publication number
EP0708174B1
EP0708174B1 EP95402302A EP95402302A EP0708174B1 EP 0708174 B1 EP0708174 B1 EP 0708174B1 EP 95402302 A EP95402302 A EP 95402302A EP 95402302 A EP95402302 A EP 95402302A EP 0708174 B1 EP0708174 B1 EP 0708174B1
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Prior art keywords
oil
line
extraction
zone
ppm
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Expired - Lifetime
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EP95402302A
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English (en)
French (fr)
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EP0708174A1 (de
Inventor
Marcel Aussillous
Patrick Briot
Pierre-Henri Bigeard
Alain Billon
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IFP Energies Nouvelles IFPEN
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IFP Energies Nouvelles IFPEN
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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
    • C10M175/0025—Working-up used lubricants to recover useful products ; Cleaning by thermal processes
    • C10M175/0033—Working-up used lubricants to recover useful products ; Cleaning by thermal processes using distillation processes; devices therefor
    • 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
    • C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
    • 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
    • C10M175/005—Working-up used lubricants to recover useful products ; Cleaning using extraction processes; apparatus therefor

Definitions

  • the present invention relates to a method and an installation for the purification of used oils, i.e. a treatment intended to produce at least one base oil usable again.
  • oils are in particular mineral oils of hydrocarbons, generally of petroleum origin, most often containing various additives such as agents anti-rust, antioxidants, emulsifiers, viscosity additives, etc., oils which after more or less long use in an internal combustion engine, as agents lubrication, have had their properties adversely changed and have loaded with products such as carbonaceous residues, oxidized products, water, hydrocarbons not burnt, which led to drain them.
  • additives such as agents anti-rust, antioxidants, emulsifiers, viscosity additives, etc.
  • Used oils contain a multitude of contaminating elements since practically all the groups of the periodic table can be represented, as the example demonstrates below.
  • Another process for regenerating used oils uses acid treatment sulfuric sections obtained during clarification with solvent or distillation under empty. These sections, freed from acid sludge, are then treated with adsorbent.
  • waste (acid sludge, adsorbents) is produced, elimination requires taking into account the ecological constraints linked to Environmental Protection. This elimination, storage and treatment is therefore expensive and increases the costs of current processes.
  • the charge of used oil (s) to be treated which has previously been freed of the particles in suspension by filtration, for example on a sieve, is introduced into the dehydration 2.
  • Dehydration techniques are those used on most regeneration chains of oils.
  • distillation is carried out at atmospheric pressure or under a slight vacuum so as not to spoil the products.
  • the distillation temperature is below 240 ° C or even less than 200 ° C, for example 120 to 180 ° C, or 120 - 150 ° C.
  • the HD dehydrated oil thus obtained is sent directly to a vacuum distillation 5, that is to say without undergoing solvent extraction as in the art prior.
  • This oil charge is brought to a high temperature so as to subject it to a suitable heat treatment so that the oil is not cracked thermally, but that the dispersing additives are destabilized.
  • the vacuum distillation column will advantageously be adjusted in order to obtain a top so-called diesel cut (GO), in lateral racking one or more so-called distillate cuts under vacuum and bottom a distillation residue.
  • GO diesel cut
  • distillate cuts under vacuum
  • bottom a distillation residue This preferred embodiment is shown on the Figure 1 with production of two vacuum distillates.
  • the diesel cut collected at the head of the column is very rich in chlorine and contains metals, mainly silicon. Its final boiling point is between 280 and 370 ° C.
  • the distilled fraction could be, for example, a spindle fraction (light oil of viscosity at 40 ° C close to 20.10 -6 m 2 / s) and engine oil bases such as SSU 100 to 600 oils.
  • a spindle fraction light oil of viscosity at 40 ° C close to 20.10 -6 m 2 / s
  • engine oil bases such as SSU 100 to 600 oils.
  • the vacuum residue contains the majority of metals and metalloids (around 6,000 - 25,000 ppm for example) present in oil and mainly polymers rushed. It corresponds to an initial boiling point of 450 to 500 ° C.
  • the vacuum residue obtained is sent to an extraction zone 9 where it is treated with preferably by means of a paraffinic hydrocarbon containing 3 to 6 carbon atoms or a mixture of several of these hydrocarbons in the liquid state, so as to extract the clarified oil from the residue.
  • the extraction treatment with light liquid paraffinic hydrocarbon is carried out preferably between 40 ° C and the critical temperature of the hydrocarbon, under pressure sufficient to maintain this hydrocarbon in the liquid state.
  • propane by example, the preferred temperature is between 45 ° C and the critical temperature of the hydrocarbon.
  • the gradient of temperature is preferably higher than 20 ° C, and better still at least 25 ° C).
  • the liquid hydrocarbon / oil volume ratio is 2: 1 to 30: 1, preferably 5: 1 to 15: 1.
  • Propane is the preferred hydrocarbon.
  • the contacting of the residue under vacuum with the light paraffinic hydrocarbon is generally carried out continuously in a column (extractor) from which firstly withdraw a mixture of paraffinic hydrocarbon and clarified oil, and on the other hand at the bottom an extraction residue R 'causing part of said hydrocarbon paraffinic.
  • the amount of solvent (paraffinic hydrocarbon) injected into the extractor is divided into two equal or unequal parts.
  • a quantity is used to dilute the charge and adjust the injection temperature of the mixture, the other part, injected directly in the column, is used to adjust the temperature at the bottom of the column and also continue to extract the oil trapped in the residue.
  • This process is very effective due to the selective dissolution of the oil in the paraffinic hydrocarbon, and the precipitation of an extremely concentrated residue at the bottom of the column.
  • the light paraffinic hydrocarbon is separated from the clarified oil HC and can then be recycled to the extraction area.
  • the solvent is separated from the oil by vaporization of the extractor head mixture on separates, by expansion and reheating followed by steam training, the hydrocarbon light clarified oil.
  • the light hydrocarbon is, after cooling, compression and condensation, advantageously recycled for a new extraction.
  • the solvent is recovered under supercritical conditions as described in patent FR-2,598,717, the teaching of which is included.
  • the separation phases is then obtained by heating, without vaporization or condensation.
  • the solvent is then recycled under supercritical pressure.
  • the advantage of these conditions supercritical is to eliminate the vaporization and condensation operations of vapors necessary in the case of conventional conditions to recover the solvent.
  • the extractor base mixture contains the residue precipitated in the hydrocarbon lightweight. This mixture has a fairly low viscosity due to the amount of light hydrocarbon it contains. Once the light hydrocarbon has been removed, its handling becomes very delicate because of the high viscosity. To overcome this drawback, the extraction residue containing solvent withdrawn at the bottom of the extractor can be mixed with a step-down viscosity. The assembly after expansion is, for example, heated and stripped with steam. The light hydrocarbon after compression and condensation, is recycled to the column extraction. The residue completely freed from the solvent can be recovered in the form of fuel or mixed with bitumen.
  • the distilled oil fraction (s) and the clarified HC oil are sent (alone or in mixture) in a hydrotreating zone 12 where they are treated with hydrogen in presence of at least one catalyst to finish purifying them and improving their qualities for better valuation.
  • This treatment makes it possible to obtain lubricating oils in accordance with the specifications. without resorting to soil treatment and / or acid treatment sulfuric. These lubricating oils have very good thermal stability and good light stability. Hydrotreatment catalyst (s) have a lifetime prolonged because the products having undergone the pre-treatment operations are well purified.
  • the catalyst is a hydrotreatment catalyst containing at least one oxide or one sulfide of at least one group VI metal and / or at least one group VIII metal, such that molybdenum, tungsten, nickel, cobalt, a support, for example alumina, silica-alumina or a zeolite.
  • a preferred catalyst is a catalyst based on nickel sulfides and molybdenum supported on alumina.
  • a final distillation allows, if necessary, to adjust the cutting points.
  • the diesel fraction obtained after vacuum distillation can also be hydrotreated to remove chlorine and lower the sulfur content. We can very advantageously mix the diesel cut with the light fractions L obtained at the dehydration by atmospheric distillation.
  • This hydrotreatment is preferably carried out with the catalysts used for the treatment of vacuum distillate (s) and clarified oil.
  • the qualities of diesel obtained at the end of this hydrotreatment make it possible to successfully pass all the specifications and allows the incorporation of this cut into fuel storage.
  • the treatment according to the present invention carried out with hydrotreatment makes it possible to maintain a good level of catalyst activity.
  • the metal content is less than 5 ppm, and the chlorine content less than 5 ppm and most often undetectable.
  • the content of aromatic polynuclear compounds (PNA) is most often of the order that of the base oils obtained by hydrorefining (of the order of 0.2-0.5% weight), it can be equal to that of refined solvent oils (furfurol for example) that is to say approximately 1.5% by weight.
  • the installation comprises as zone (2) a distillation atmospheric or under light vacuum with separation of the light fraction (s) L containing petrol by a pipe (13).
  • a pipe (6) for evacuating the diesel cut from the distillation zone (5) under vacuum.
  • the diesel, distilled oil and clarified oil fractions can be processed directly by hydrotreatment in zone (12) (representation of FIG. 1), it being understood that they are treated separately.
  • they will be stored separately and processed by campaign.
  • Hydrogen is introduced into the hydrotreating zone (12) directly into the reactor (as in Figure 1) but it can be introduced with the load to be treated.
  • the invention includes this possibility.
  • a heat exchanger is advantageously arranged to cool the residue.
  • This means is preferably a means of vaporization. It is advantageously composed of at least one regulator, one heating means and a steam drive device (stripper).
  • the solvent recovered then preferably passes through a heat exchanger, a compressor and a condenser before being recycled for extraction by a pipeline suitable which connects said separation means and the extraction zone (9).
  • it is arranged in the area (9) under conditions supercritical, a heating means to separate the solvent and a pipe to recycle the solvent to zone (9).
  • the water removed by atmospheric distillation represents 4% by weight of the charge and the light fraction L 2.4% by weight.
  • the dehydrated oil (93.6% of the charge) is sent to the vacuum distillation unit: in the example chosen, we have grouped the two distillates from the side draws.
  • the 1 + 2 distillates correspond to boiling points between 280 ° C and 565 ° C.
  • the 1 + 2 distillates are sent to the hydrotreating unit, the vacuum residue is sent to the solvent clarification unit (extraction zone (9)).
  • the bottom cut (vacuum residue) obtained during vacuum distillation is sent to the solvent extraction unit.
  • the residue obtained is "fluxed" (mixed with dehydrated oil or with a hydrocarbon viscosity reducer) and can be used as fuel or used as a binder in road bitumens.
  • the clarified oil is separated from the light hydrocarbon by vaporization to give the Bright Stock (BS) cut.
  • the mixture of vacuum distillates 1 + 2 and the oil (Bright Stock) are sent respectively (separately) to the hydrotreating unit on a catalyst containing nickel sulfide, molybdenum sulfide and an alumina support.
  • the operating conditions are as follows: Temperature 300/280 ° C Partial hydrogen pressure 50 bar Residence time 1 hour Hydrogen recycling 380 Nm 3 / m 3 of load.
  • the products obtained after hydrotreatment are characterized by a reduction heavy aromatics content, a significant decrease in sulfur content, and by a total elimination of chlorine and metals.
  • the viscosity index of these bases of oils is maintained or improved, stability in the presence of heat or light is very good.
  • the extraction unit is therefore very well suited for treating the residue cut under vacuum and for the more it requires an investment divided by 3 compared to the investment of a total oil clarification installation after dehydration, since the capacity to the unit is reduced to about a third of that required in the prior art.
  • the metals contained in the clarified oil are in an amount greater than 300 ppm.
  • the molecules containing the metals (impurities) easily precipitate in the solvent medium, the high concentration of metals (degraded additives) makes it possible to have insoluble micelles which will grow in size as they grow stay in the column and by density difference fall to the bottom of the extractor.
  • the present invention which has demonstrated and exploited this effect, makes it possible to enhance the maximum all the products contained in the used oil collected.
  • the yield in recoverable products is close to 99% compared to the amount of hydrocarbon contained in the oil collected.
  • the residue leaving the extraction is itself recoverable.

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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)
  • Combustion & Propulsion (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Lubricants (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Fats And Perfumes (AREA)

Claims (14)

  1. Verfahren zur Reinigung eines verbrauchten Öls die Stufen der Dehydratisierung, der Vakuumdestillation, der Lösungsmittelextraktion und des Hydrotreatments umfassend, dadurch gekennzeichnet, dass
    das verbrauchte dehydratisierte Öl direkt unter Vakuum zur Erzeugung eines Rückstands und wenigstens einer destillierten Ölfraktion destilliert wird,
    der Vakuumdestillationsrückstand direkt dieser Extraktion derart ausgesetzt wird, dass ein sogenanntes geklärtes oder gereinigtes Öl und ein Extraktionsrückstand erhalten wird, und
    die Fraktion (die Fraktionen) des destillierten Öls und des geklärten oder gereinigten Öls einer Stabilisierungsbehandlung durch Hydrotreatment unterzogen wird (werden).
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die verbrauchten Öle durch atmosphärische Destillation bei einer Temperatur von weniger als 240°C dehydratisiert werden.
  3. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass der Vakuumdestillationsrückstand einen Anfangssiedepunkt zwischen 450 und 500°C aufweist.
  4. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Vakuumdestillation einen sogenannten Gasölschnitt mit einem Siedeendpunkt zwischen 280 und 370°C erzeugt.
  5. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Extraktion vermittels eines paraffinischen Kohlenwasserstoffs, der 3 bis 6 Kohlenstoffatome hat, bei einer Temperatur zwischen 40°C und der kritischen Temperatur des Kohlenwasserstoffs unter einem ausreichenden Druck durchgeführt wird, um den Kohlenwasserstoff im flüssigen Zustand zu halten, und dies bei einem Volumenverhältnis Kohlenwasserstoff/ÖI zwischen 2 : 1 und 30:1.
  6. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Extraktion mit Propan durchgeführt wird.
  7. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die aus der Extraktion stammende Fraktion, welche das geklärte Öl enthält und auch Lösungsmittel enthält, einer Verdampfung derart ausgesetzt wird, dass das Lösungsmittel, welches zur Extraktion rezykliert wird, abgetrennt wird.
  8. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass das Lösungsmittel vom geklärten oder gereinigten Öl unter überkritischen Bedingungen getrennt wird und dass es zur Extraktion unter einem überkritischen Druck rezykliert wird.
  9. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass der Extraktionsrückstand mit einem Viskositätssenker vermischt wird.
  10. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass der (die) Gasölschnitt(e) ebenfalls einem Hydrotreatment ausgesetzt wird (werden).
  11. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass das Hydrotreatment unter Wasserstoff in Anwesenheit eines Katalysators durchgeführt wird, der über einen Träger verfügt und wenigstens ein Oxid oder ein Sulfid wenigstens eines Metalls der Gruppe VI und/oder wenigstens eines Metalls der Gruppe VIII bei einer Temperatur von 250 - 400°C, einem Druck von 5 - 150 bar und einer Raumgeschwindigkeit von 0,1-10h-1 stattfindet.
  12. Installation zur Durchführung des Verfahrens nach einem der Ansprüche 1 bis 11, umfassend:
    eine Zone (2) zur Dehydratation, verbunden mit einer Leitung (1) zum Einführen der Charge des verbrauchten Öls, einer Leitung. (3) zum Austritt des Wassers und einer Leitung (4) zum Abzug des dehydratisierten Öls,
    eine Zone (5) zur Vakuumdestillation, in welche die Leitung (4) mündet und die wenigstens mit einer Leitung (7) zum Abzug der Fraktion (der Fraktionen) des destillierten Öls und wenigstens einer Leitung (8) zum Abzug des Vakuumrückstands versehen ist,
    eine Zone (12) des Hydrotreatments, versehen mit wenigstens einer Leitung (7, 10, 13) zum Einführen des zu behandelnden Schnitts, wenigstens einer Leitung zum Abziehen des behandelten Schnitts (16, 17), wenigstens einer Leitung (14) zum Zuführen von Wasserstoff und wenigstens einer Leitung (15) für den Gasaustritt,
    eine Zone (9) zur Lösungsmittelextraktion,
    wobei diese Installation sich dadurch auszeichnet, dass
    eine Leitung (4) aus der Dehydratisierungszone (2) das dehydratisierte Öl abzieht und es direkt in die Zone (5) der Vakuumdestillation gibt, und dass
    die Extraktionszone (9) mit einer Leitung (18) zum Einführen des Lösungsmittels, einer Leitung (8) zur direkten Zuführung des Rückstands aus der Vakuumdestillationszone (5) zur Zone (9), einer Leitung (11) zum Abzug des Extraktionsrückstands und einer Leitung (10) für den Austritt des geklärten oder gereinigten Öls versehen ist.
  13. Installation nach Anspruch 12, dadurch gekennzeichnet, dass die Zone 2 der Dehydratation durch Destillation versehen ist mit einer Leitung (13) für den Austritt der leichten Fraktion, welche das Benzin enthält, und dass eine Leitung (6) aus der Vakuumdestillationszone (5) den Gasölschnitt abzieht.
  14. Installation nach einem der Ansprüche 12 oder 13, dadurch gekennzeichnet, dass in Höhe der Zone (9) ein Mittel zum Trennen des Lösungsmittels vom gereinigten Öl angeordnet ist, und dass eine Rezyklierungsleitung für das Lösungsmittel dieses Trennmittel und die Extraktionszone (9) verbindet.
EP95402302A 1994-10-17 1995-10-16 Verfahren und Anlage zur Reinigung von Altölen Expired - Lifetime EP0708174B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9412448A FR2725725B1 (fr) 1994-10-17 1994-10-17 Procede et installation pour la purification des huiles usagees
FR9412448 1994-10-17

Publications (2)

Publication Number Publication Date
EP0708174A1 EP0708174A1 (de) 1996-04-24
EP0708174B1 true EP0708174B1 (de) 2001-12-12

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US (2) US5759385A (de)
EP (1) EP0708174B1 (de)
JP (1) JP4051488B2 (de)
KR (1) KR100372802B1 (de)
CN (1) CN1100854C (de)
CA (1) CA2160652C (de)
DE (1) DE69524533T2 (de)
EG (1) EG20615A (de)
ES (1) ES2169748T3 (de)
FR (1) FR2725725B1 (de)
NO (1) NO313296B1 (de)
PL (1) PL177602B1 (de)
SA (2) SA95160353B1 (de)

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CN1128789A (zh) 1996-08-14
EG20615A (fr) 1999-09-30
JPH08199185A (ja) 1996-08-06
SA95260105B1 (ar) 2006-06-04
ES2169748T3 (es) 2002-07-16
EP0708174A1 (de) 1996-04-24
US5759385A (en) 1998-06-02
DE69524533D1 (de) 2002-01-24
KR960014307A (ko) 1996-05-22
JP4051488B2 (ja) 2008-02-27
NO954097L (no) 1996-04-18
PL177602B1 (pl) 1999-12-31
CA2160652A1 (fr) 1996-04-18
NO313296B1 (no) 2002-09-09
CA2160652C (fr) 2007-10-09
FR2725725A1 (fr) 1996-04-19
PL310964A1 (en) 1996-04-29
KR100372802B1 (ko) 2003-04-26
DE69524533T2 (de) 2002-05-29
US5843384A (en) 1998-12-01
SA95160353B1 (ar) 2006-06-04
NO954097D0 (no) 1995-10-13
FR2725725B1 (fr) 1996-12-13
CN1100854C (zh) 2003-02-05

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