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EP3098290A1 - Procédé pour la régénération des huiles utilisées - Google Patents

Procédé pour la régénération des huiles utilisées Download PDF

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Publication number
EP3098290A1
EP3098290A1 EP16164483.6A EP16164483A EP3098290A1 EP 3098290 A1 EP3098290 A1 EP 3098290A1 EP 16164483 A EP16164483 A EP 16164483A EP 3098290 A1 EP3098290 A1 EP 3098290A1
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EP
European Patent Office
Prior art keywords
fraction
quality
oil
plant
regenerated
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
EP16164483.6A
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German (de)
English (en)
Other versions
EP3098290B1 (fr
Inventor
Francesco Gallo
Alessandro QUAGLIA
Maurizio GIUSTI
Aldo ROLDI
Danilo DE ARCANGELIS
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.)
Viscolube Srl
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Viscolube Srl
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Priority to PL16164483T priority Critical patent/PL3098290T3/pl
Publication of EP3098290A1 publication Critical patent/EP3098290A1/fr
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Publication of EP3098290B1 publication Critical patent/EP3098290B1/fr
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Classifications

    • 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
    • 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
    • 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
    • C10M175/0041—Working-up used lubricants to recover useful products ; Cleaning by thermal processes by hydrogenation processes
    • 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
    • C10M175/0058—Working-up used lubricants to recover useful products ; Cleaning by filtration and centrifugation processes; apparatus therefor
    • 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
    • C10M175/06—Working-up used lubricants to recover useful products ; Cleaning by ultrafiltration or osmosis

Definitions

  • the present invention relates to a regeneration process for waste oils, in particular mineral oils, aimed at achieving the enhancement of the same oils, with a lower power consumption compared to conventional processes.
  • Lubricating oils have been used for a very long time in almost all the fields of mechanics to allow engine parts or the like to slide on each other.
  • a classic example is that of oil used in internal combustion engines to help the sliding of the pistons in the cylinders, without the mechanical parts getting stuck into one another.
  • Lubricating oils are often used in machinery involving very fast relative sliding movements of their parts. Because of this, in addition to other aspects, lubricating oils frequently undergo temperature changes, which are in some cases remarkable. For this reason, oils undergo chemical reactions of various kinds and their nature is altered. As a consequence, reactions such as cleavage, dehydration, dehydrogenation, condensation, etc. take place. An example of such a reaction is the dehydrogenation-dehydration of oils, which leads to the formation of carbon in the form of carbon black. In some cases, the formation of asphaltenes and bitumens also occurs. Furthermore, the oils can contact other substances, such as, for example, metallic and/or ceramic particles, thus remaining inside the oil itself.
  • Waste oil normally contains a number of toxic substances, for which reason it cannot be simply discharged into the environment, but must be treated to reduce its environmental impact. The regeneration of waste oils has thus emerged as a solution allowing to reduce waste and the resulting environmental impact.
  • the typical yield of a regeneration process starting from 100 kg of waste oil to be sent to the process, is now always around 60 kg of regenerated oil (base for lubricants), 20-25 kg of fuel and 20-25 kg of bitumen.
  • the step of acid treatment is completely replaced by clarification with liquid propane.
  • the chosen hydrocarbon is propane for being easily liquefiable and having a low density once liquefied. It therefore acts as fluidifying agent on oils to which it is added, so as to allow the separation of a high-density phase - containing high molecular weight polymers and heavy metals - from a second fraction, constituted by clarified and dehydrated oils.
  • the propane is then removed and recycled by mixing with the in-fed oils.
  • a hot filtration is then performed, allowing the recovery of a gaseous fraction. Discoloration and deodorisation of the content are the final steps.
  • EP 0 618 959 discloses a process for re-refining waste oils, in which said oils are contacted with a basic reagent and heated to remove contained water, polymers and heavy metals are separated and fractioned distillation is performed in a packed column, in order to obtain one or more base fractions for lubricant, followed by discoloration.
  • the basic reagent is a strong base, water is removed together with a more volatile fraction in a preliminary step of flash distillation, while polymers and heavy metals are removed mostly by decanting.
  • the packed distillation column tends to become clogged by solid residues, still contained in the oil to be fed inside the same.
  • the flash distillation column entails high operating costs.
  • WO2004/033 608 discloses a process and a device for the treatment of waste oils, which includes a preliminary separation by decanting of at least one fraction of the water and one fraction of solid particles (sediments), a pre-heating of the oily phase from the decanting step and centrifugal separation of the oil, preheated to a temperature below the boiling point of water, followed by the separation of water and other pollutants.
  • the product obtained is not reused to produce new lubricant bases, but is fed to a combustion step, along with other hydrocarbons, therefore with no enhancement of the same.
  • WO96/00 273 discloses a process of reclamation of waste oils, with a view to their reuse. According to this document, waste oil undergoes a centrifugation as it is to remove solid matters; the output oil is then contacted with diammonium phosphate and/or oxalic acid at a temperature between 60 and 85-90°C and is then subjected to a new centrifugation to separate oil and water. There are no distillation steps.
  • FR 2 787 118 discloses the recovery of high value-added additives, while enhancing the distillation tails, resulting in a high viscosity index oil by low-temperature fractioned distillation.
  • DE 2 605 484 discloses a process for making waste mineral oil reusable, which involves heating the oil to a temperature of 204-427°C, at a pressure between 35,2 and 246 kg/cm 2 and thereafter separating the foam that forms.
  • DE 69 524 533 relates to a process for the purification of a waste mineral oil, comprising the steps of dehydration, vacuum distillation, solvent extraction and hydrorefining.
  • Dehydrated oil is directly distilled under vacuum; the distillation tail is subjected to extraction with solvents; the output from these treatments is subjected to hydrorefining.
  • JP 1988 0 291 191 describes a treatment process of oily residues in a steel mill, involving grinding of steel mill residues separated from oil and their combustion to produce ferric oxide.
  • the object of the present invention is to propose a process allowing to obtain lubricant bases and good quality bitumen, possibly reducing the required power consumption, thus overcoming the drawbacks of the prior art.
  • This task is achieved, according to the present invention, by a process for the regeneration of waste oils, which provides a fractioned distillation in a packed column and hydrorefining of the oil and the grinding of sediments, characterised in that the oil to be regenerated is fed divided into two separate fractions, a better-quality one and a lower-quality one containing more impurities, said better-quality fraction undergoing flash distillation, centrifugation and dehydration, to be subsequently sent to the distillation packed column, while said worse-quality fraction undergoes homogenisation, grinding and decanting, the liquid phase which is obtained following these processes being mixed with the better-quality fraction and the solid phase being recycled to the homogenisation step.
  • the subclaims disclose further preferred embodiments.
  • a first embodiment of the present invention is represented in fig. 1 .
  • the oil to be regenerated is divided, at the time of acquisition, into two fractions, a better-quality one and a worse-quality one.
  • the worse-quality fraction contains substantial quantities of foreign matter, such as, for example, polymers and similar pollutants, while the better-quality fraction exhibits a low or even negligible content of solid matter, such solid substances being mostly carbon residues, related to oil impairing in its use.
  • the better-quality oil fraction to be regenerated has a total sediment of a maximum of 3% by volume, a minimum viscosity at 50°C of 1.8°E, a maximum sulphur content of 1.5% by mass, while the worse-quality oil fraction to be regenerated has a total sediment in an amount greater than 3% by volume, a minimum viscosity at 50°C of 1°E and a maximum sulphur content equal to 3% by mass.
  • the worse-quality fraction is fed to the plant at 1, while the better-quality fraction is fed at 2.
  • the fraction 1 then enters a mixer 3.
  • the mixer 3 mixes and homogenises the incoming oil, so as to disperse the impurities within it in a uniform manner, thus reducing to a minimum the possible phase separations. In view of this, it is possible to arrange an emulsion treatment.
  • the mixed and homogenised fraction output from the mixer 3 is sent to a grinding device 5 through pipeline 4.
  • the grinding device 5 can be of any known type. Instruments such as ball mills and wedge mills are preferred.
  • said grinding device 5 is a ball mill, easy to use and allowing to achieve excellent results.
  • the device 5 breaks and opens solid particles contained in the oil to be regenerated, thus making available more oil, contained within the particles themselves.
  • a pipeline 6 sends the ground fraction to a decanter 7.
  • the better-quality fraction 2 it is, first, fed to a flash distillation column 10.
  • the column 10 is operated at a pressure of about 250 torr and a temperature of about 130-140°C, slightly higher than the water boiling temperature, to remove as much water as possible from the oil to be regenerated.
  • the aqueous fraction leaves the column 10 through the outlet 11. Instead, the fraction containing the oil to be regenerated comes out of the pipeline 12, in which the liquid from the pipeline 8 flows, and is fed to a centrifugal separator 13.
  • the centrifugal separator 13 outputs two flows: a flow 14, containing mostly solids sediment, which is sent to the mixer 3, and a second flow 15, containing the fluid to be regenerated, that is sent to a dehydration unit 16.
  • the oil to be regenerated inside the pipeline 18, before being subjected to fractioned distillation, can optionally be subjected to adjustment of its viscosity, according to processes known per se to the person skilled in the art, thus improving its commercial impact.
  • the pipeline 18 is fed to a heat exchanger 19, preferably an oven, bringing the oil temperature to a value higher than 300°C, preferably to a value between 350 and 400°C.
  • the oil to be regenerated can be sent to a further centrifugal separator, not shown in the figures.
  • the sediments output from this additional centrifugation step are preferably sent to the mixer 3.
  • a pipeline 20 carries the heated oil to a packed distillation column 21, where fractioned distillation of the oil is performed.
  • the pressure inside the column 21 is adjusted, preferably, to a value ranging from 8 to 15 torr.
  • pressure is adjusted by a liquid-ring pump, allowing to reduce the clogging of the packing.
  • the tail of the column 21 produces a fraction 22, containing mostly bitumen, which can be sold or used as such.
  • Column 21 also outputs head fractions 23 and intermediate fractions 24, 25 and 26.
  • the fractions 23, 24, 25 and 26 are then sent to a reactor 27, where a hydrorefining step is performed, yielding the desired lubricant bases, output at 28.
  • the reactor 27 is normally operated at a pressure above 80 bar. The fact of having separated the best and worst fractions at the beginning and having ground the sediment output from the decanter 7 and from the centrifugal separator 13 ensures that, with the process according to the present invention, one can obtain similar or even better results managing the reactor 27 at a pressure of about 60 bars, which implies a considerable power saving.
  • the fraction 23, either subjected to hydrorefining or as it is, can be used within the system to operate a cogeneration engine that provides electric power and steam to the entire system.
  • the water from the plant for example in 11 and 17, can be subjected to an oxidation treatment of its pollutants with wet air (technique known as wet air oxidation), thus allowing to recover steam, to be used in the plant.
  • wet air oxidation oxidation treatment of its pollutants with wet air
  • FIG. 2 An alternative embodiment of the present invention is represented in fig. 2 . Components identical to those of the previous embodiment will carry the same reference numerals. The operating parts identical to those of the embodiment of Fig. 1 will not be described again to avoid encumbering the reading and, for them, it is possible to refer to what previously reported.
  • bitumen leaving the packed distillation column 21 through the pipeline 22, instead of being used or sold as such, is subjected to an enhancement process, which also has the effect to further push the yield in the lubricating bases produced.
  • the pipeline 22 carries the bitumen to a mixer 29, which homogenises the bitumen.
  • the bitumen comes out through a pipeline 30 and is fed by it to a grinding device 31, completely analogous to the mixing device 5, already seen previously.
  • the liquid fraction consisting of a more valuable bitumen which can be used for more refined uses than normal, as for the production of inks, comes out in 32, while the solid fraction is re-fed to the mixer 3, along with the other sediment and to the fraction 1, containing the oil of worse quality to be regenerated.
  • FIG. 3 Another alternative embodiment is illustrated in Fig. 3 . Even in this case, parts identical to those of the preceding embodiments have identical reference numerals. Even in this case, the common part of the description is omitted to avoid burdening the discussion.
  • Fractions 23, 24, 25 and 26, output from the packed distillation column 21, are fed to a tank 34 which acts as a buffer, to allow the subsequent operations to be carried out discontinuously, load-wise or batch-wise.
  • a pipeline 35 feeding a microfiltration unit 36 exits from the tank 34. Two flows are output by this unit.
  • a pipeline 37 sends the oil fraction to the hydrorefining reactor 27, from which the produced lubricant bases will exit.
  • a pipeline 38 removes the solid sediments from the unit.
  • the pipeline 38 instead of the waste, can bring sediments to the mixer 3, increasing the quality of bitumen produced and its yield. Therefore, between the step of fractional distillation in a packed column and the step of hydrorefining, a microfiltration step of the oil in regeneration is provided.
  • the present invention allows to achieve important power savings, obtaining high yields and extremely clean products of high value.
  • not all the oil to be regenerated is subjected to flash distillation, but only the better quality fraction.
  • the column 10 can be of relatively small size and requires less power for its operation compared to the power that would be required to submit all the oil to be regenerated to flash distillation.
  • the pressure within the hydrorefining reactor is maintained much lower for the same performance, resulting in a lower power consumption for the maintenance of pressure.
  • the present invention also relates to a plant for the implementation of the process, this plant comprising a packed distillation column 21 and a reactor 27 for hydrorefining, characterised in that it has two feeds 1 and 2 of oil to be regenerated, a worse-quality fraction being fed to one (1) of said feeds 1, 2 and a better-quality fraction being fed to the other (2) of said feeds 1, 2 and in that it further comprises at least a grinding device 5 for grinding solid sediments through which the worse-quality fraction passes after the feed 1, and after passing through a mixer 3 and at least one centrifugal separator 13, in which a fraction 12 is fed, consisting of the oil fraction to be regenerated, coming from the better-quality feed 2 output by a flash distillation column 10, which is mixed with the part floating in a decanter 7 which received the fraction ground in the device 5.
  • this plant comprising a packed distillation column 21 and a reactor 27 for hydrorefining, characterised in that it has two feeds 1 and 2 of oil to be regenerated, a worse

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Fats And Perfumes (AREA)
EP16164483.6A 2015-05-28 2016-04-08 Procédé pour la régénération des huiles utilisées Active EP3098290B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL16164483T PL3098290T3 (pl) 2015-05-28 2016-04-08 Sposób regeneracji olejów odpadowych

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
ITUB2015A000917A ITUB20150917A1 (it) 2015-05-28 2015-05-28 Processo per la rigenerazione di olii usati

Publications (2)

Publication Number Publication Date
EP3098290A1 true EP3098290A1 (fr) 2016-11-30
EP3098290B1 EP3098290B1 (fr) 2017-12-06

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EP16164483.6A Active EP3098290B1 (fr) 2015-05-28 2016-04-08 Procédé pour la régénération des huiles utilisées

Country Status (6)

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EP (1) EP3098290B1 (fr)
ES (1) ES2661316T3 (fr)
HU (1) HUE036574T2 (fr)
IT (1) ITUB20150917A1 (fr)
PL (1) PL3098290T3 (fr)
PT (1) PT3098290T (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108547200A (zh) * 2018-06-07 2018-09-18 福建南方路面机械有限公司 沥青路面废料再生系统及再生方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT201900015626A1 (it) 2019-09-05 2021-03-05 Certech S P A Con Socio Unico Mulino continuo a livello controllabile

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2605484A1 (de) 1975-04-24 1976-11-11 Witco Chemical Corp Verfahren zum wiederverwendbarmachen von gebrauchten kurbelgehaeuseoelen
JPH02145437A (ja) * 1988-11-28 1990-06-04 Mitsubishi Heavy Ind Ltd 鉄分を含有する石油スラッジの処理方法
EP0618959A1 (fr) 1992-09-30 1994-10-12 Viscolube Italiana S.P.A. Procede de reraffinage d'huiles usees
WO1996000273A1 (fr) 1994-06-23 1996-01-04 Corex Technologies (1993) Ltd. Procede de recuperation d'huiles lubrifiantes usees
FR2787118A1 (fr) 1998-12-09 2000-06-16 Richard Deutsch Procede de recuperation des huiles de synthese et d'elaboration d'huiles a haut indice de viscosite a partir d'huiles de lubrification usagees
DE69524533T2 (de) 1994-10-17 2002-05-29 Institut Francais Du Petrole, Rueil-Malmaison Verfahren und Anlage zur Reinigung von Altölen
WO2004033608A1 (fr) 2002-10-10 2004-04-22 Totalfinaelf France Procede et dispositif pour le traitement d'huiles lubrifiantes usagees.

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2605484A1 (de) 1975-04-24 1976-11-11 Witco Chemical Corp Verfahren zum wiederverwendbarmachen von gebrauchten kurbelgehaeuseoelen
JPH02145437A (ja) * 1988-11-28 1990-06-04 Mitsubishi Heavy Ind Ltd 鉄分を含有する石油スラッジの処理方法
EP0618959A1 (fr) 1992-09-30 1994-10-12 Viscolube Italiana S.P.A. Procede de reraffinage d'huiles usees
WO1996000273A1 (fr) 1994-06-23 1996-01-04 Corex Technologies (1993) Ltd. Procede de recuperation d'huiles lubrifiantes usees
DE69524533T2 (de) 1994-10-17 2002-05-29 Institut Francais Du Petrole, Rueil-Malmaison Verfahren und Anlage zur Reinigung von Altölen
FR2787118A1 (fr) 1998-12-09 2000-06-16 Richard Deutsch Procede de recuperation des huiles de synthese et d'elaboration d'huiles a haut indice de viscosite a partir d'huiles de lubrification usagees
WO2004033608A1 (fr) 2002-10-10 2004-04-22 Totalfinaelf France Procede et dispositif pour le traitement d'huiles lubrifiantes usagees.

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Week 199028, Derwent World Patents Index; AN 1990-214349, XP002751241 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108547200A (zh) * 2018-06-07 2018-09-18 福建南方路面机械有限公司 沥青路面废料再生系统及再生方法

Also Published As

Publication number Publication date
HUE036574T2 (hu) 2018-07-30
PT3098290T (pt) 2018-02-13
ES2661316T3 (es) 2018-03-28
EP3098290B1 (fr) 2017-12-06
PL3098290T3 (pl) 2018-05-30
ITUB20150917A1 (it) 2016-11-28

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