EP3392328B1 - Process for the regeneration of exhaust oils - Google Patents

Process for the regeneration of exhaust oils Download PDF

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Publication number
EP3392328B1
EP3392328B1 EP18166609.0A EP18166609A EP3392328B1 EP 3392328 B1 EP3392328 B1 EP 3392328B1 EP 18166609 A EP18166609 A EP 18166609A EP 3392328 B1 EP3392328 B1 EP 3392328B1
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EP
European Patent Office
Prior art keywords
hydro
refining
oils
regeneration
exhaust
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.)
Active
Application number
EP18166609.0A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP3392328A1 (en
Inventor
Francesco Gallo
Alessandro QUAGLIA
Aldo ROLDI
Maurizio GIUSTI
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Itelyum Regeneration SpA
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Itelyum Regeneration SpA
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Priority to PL18166609T priority Critical patent/PL3392328T3/pl
Publication of EP3392328A1 publication Critical patent/EP3392328A1/en
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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
    • 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

Definitions

  • the present invention refers to a process for the regeneration of exhaust oils, in which the silicon sources are removed.
  • Lubricating oils have been used for a very long time in almost all the fields of mechanics to facilitate the mutual sliding of engine parts or the like.
  • 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 having 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, oils can contact other substances, such as, for example, metallic and/or ceramic particles, thus remaining inside the oil itself.
  • Exhaust oil normally contains a number of substances toxic for the humans and the environment, for which reason it cannot be simply discharged into the environment, but it must be appropriately treated so as to reduce its environmental impact. The regeneration of exhaust 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 exhaust oil to be sent to the process, is now 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. Propane is then removed and recycled by mixing it with the in-fed oils.
  • a hot filtration is then performed, allowing the recovery of a gaseous fraction. Discolouration and deodorisation of the content close the process.
  • 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 discolouration.
  • 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 partial vaporisation distillation column entails high operating costs.
  • WO2004/033 608 discloses a process and a device for the treatment of exhaust oils, which includes a preliminary separation by decanting of at least one fraction of the water and one fraction of solid particles (sediments), a preheating 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 exhaust oils, with a view to their reuse. According to this document, exhaust oil undergoes a centrifugation as it is to remove solids; 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.
  • EP-A-3 098 291 discloses a process for the regeneration of waste oils, comprising a flash distillation step of the oil to be regenerated, a decanting step of the heavy fraction, a distillation step in a packed distillation column, allowing to produce an oil fraction to be sent to hydrorefining and a bitumen fraction.
  • the bitumen fraction is ground, the liquid fraction obtained after grinding being separated and collected as bitumen and the remaining solid fraction being separated and recycled to said step of decanting of the heavy fraction.
  • the lubricating bases that are obtained from the regeneration processes of exhaust oils and which provide a hydro-refining unit of the oils produced, before their use.
  • the lubricating bases obtained contain around 50 mg/l of silica, i.e., they have a silicon content much higher than that allowed by the regulations and, thus, a removal of the silica becomes mandatory in order to put on the market the product obtained from the regeneration.
  • the underlying problem of the invention is to propose a process and a regeneration plant of exhaust oils which overcomes the above mentioned drawbacks and which allows to obtain as a main product, bases for lubricants with zero or low silicon content.
  • this object is achieved through a process for the regeneration of exhaust oils, comprising a fractional distillation step and a hydro-refining step, characterised in that the hydrogen supplied during the hydro-refining step comes from the reforming of biogas, and in that the hydrogen recycled following after hydro-refining undergoes desiloxanation before being reintroduced into the hydro-refining reactor.
  • the object is achieved through a plant for the regeneration of exhaust oils, comprising a column for fractional distillation and a hydro-refining reactor of the fractions leaving said fractional distillation column, wherein the outgoing product is separated into product and recycled matter, the latter consisting mainly of unreacted hydrogen, characterised in that said recycled matter is sent back to the hydro-refining reactor after having run through a desiloxanation unit and in that the hydrogen supplied during the hydro-refining step comes from the reforming of biogas.
  • Fig. 1 shows, in an extremely general and schematic way, a plant for the regeneration of exhaust oils, of the type that can be used to put implement the process according to the present invention.
  • the plant comprises a feeding 1, from which the exhaust oils, as they come from the collection and possibly mixed with alkalis and pre-stirred, are fed. It is possible that the oils fed in 1 have already undergone some pre-treatments, of which, however, it is not considered necessary to further discuss here, because, although certainly useful for the quality of the product that can be obtained, such treatments, however, do not affect the present invention.
  • the feeding 1 is connected to a flash distillation column 2.
  • the column 2 mainly serves to remove a large part of the pollutants contained in the oil to be regenerated, in particular water and contaminants dissolved therein or mixed therewith.
  • the column 2 comprises two outlet ducts, 3 and 4.
  • the duct 4 is connected to a fractional distillation column 5.
  • a member of flows come out from column 5.
  • the duct 6 is an exhaust duct, mainly containing bitumen, while the ducts 7, 8 and 9 are connected to a hydro-refining reactor 10.
  • the ducts 11, 12 and 13 come out of the column 10, which contain the bases for lubricants which constitute the desired product.
  • Fig. 2 the hydro-refining reactor 10 is shown, for simplicity, fed by the duct 9 alone and with the outlet duct 13 alone; the arguments that will be referred below can also be applied to the ducts not shown, but still present in the system.
  • the duct 13 coming from the reactor 10 leads to a liquid-gas separator 14.
  • the separator 14 has a drain 15 and a recycled 16.
  • a desiloxanation unit 17 is inserted on the recycled 16. The recycle 16 continues until it converges into the feeding 9.
  • the feeding 1 is sent to a flash distillation column 2, operating at a temperature just above the boiling temperature of the water, preferably at about 140°C. Low pressure is maintained, generally around 250 torr. From column 2, water vapour flows through the duct 3, which is created by evaporation of the water contained in the oil to be regenerated, while the oil to be further regenerated flows through the duct 4, from which it is brought in known manner to a temperature higher than 300°C, thus being fed to the fractional distillation column 5.
  • the bitumen by-product comes from the duct 5, which can be further treated in a manner known per se for its valorisation, while the product to be regenerated comes from the ducts 7, 8 and 9; the ducts 7, 8 and 9 themselves feed this product to be regenerated to the hydro-refining column 10, from which, through the ducts 11, 12 and 13, the bases for lubricants come out, which are the product of the process according to the invention.
  • Possible microfiltration units can be provided downstream of the hydro-refining reactor 10, to further push the regeneration and obtain an even higher quality product.
  • the hydro-refining takes place at a temperature between 260 and 360°C, at a pressure of about 100 bar and in the presence of a catalyst based on NiMoO 4 .
  • the hydrogen fed in the hydro-refining step comes from the reforming of biogas.
  • the hydrogen obtained from this source allows to reduce the environmental impact linked to its production.
  • the products come from the reactor 10 through the ducts 11, 12 and 13. They are fed to the liquid-gas separator 14.
  • the liquid flow 15 is sent for sale as a product, while the flow 16, containing mostly unreacted hydrogen, is sent to the desiloxanation unit 17.
  • the siloxane is removed from the gas flow, which, thus, remains purified.
  • the removal of the siloxane can take place by means of activated carbons, anaerobic digestion, regenerative filtration, microemulsion, or by other techniques, mostly known per se.
  • the gas hydrogen which is thus recycled to the reactor 10 contains less siloxane than at the beginning.
  • a siloxane and not another siliceous compound is removed, because it has been found that the silica found in the lubricating bases constituting the final product of these processes comes mainly from the transformation of siloxane into silica.
  • the arrangement of the desiloxanation unit 17 on the recycling of the unreacted hydrogen inside the duct 16 has advantages which are not imaginable per se in the light of the current state of the art. In fact, one could think of placing the aforementioned unit on the effluent of the product (15). In this way, the product would have a silicon content lower than the allowed limits, so that it can be easily sold without further treatments to remove silicon. However, the arrangement of the unit 17 on the duct 16 causes the hydrogen to be fed to the reactor 10 to contain a lower silicon concentration than is normally the case.
  • the silicon that is at the end of conventional regeneration processes contains silica obtained by transformation of siloxane and it seems that the siloxane is introduced into the regeneration cycle by hydrogen, especially if it comes from reforming of biogas, which contains from 1500 to 4000 mg/l; normally, this type of hydrogen is used for its reduced environmental impact, but, as mentioned above, the siloxane content is higher than in the hydrogen obtained from other sources.
  • the unit 17 is arranged on the recycle duct avoids the hydrogen recycled to the reactor 10 from containing only negligible amounts of siloxane and its mixing with the fresh hydrogen thus allows to introduce into the reactor 10 a quantity lower than the normal siloxane, so as to allow a longer duration of the catalyst based on NiMoO 4 .
  • there is a more pure product (containing less silica), with a much longer duration of the life of the catalyst based on NiMoO 4 with a consequent economic advantage that is not negligible, as, in addition to a lower purchase price and activation of the catalyst, there are less downtime of plant shutdown, with a not negligible increase in productivity.

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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)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
EP18166609.0A 2017-04-19 2018-04-10 Process for the regeneration of exhaust oils Active EP3392328B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL18166609T PL3392328T3 (pl) 2017-04-19 2018-04-10 Proces regeneracji olejów odpadowych

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
IT102017000042853A IT201700042853A1 (it) 2017-04-19 2017-04-19 Processo per la rigenerazione di olii usati

Publications (2)

Publication Number Publication Date
EP3392328A1 EP3392328A1 (en) 2018-10-24
EP3392328B1 true EP3392328B1 (en) 2019-09-18

Family

ID=59700113

Family Applications (1)

Application Number Title Priority Date Filing Date
EP18166609.0A Active EP3392328B1 (en) 2017-04-19 2018-04-10 Process for the regeneration of exhaust oils

Country Status (5)

Country Link
EP (1) EP3392328B1 (pl)
ES (1) ES2753275T3 (pl)
IT (1) IT201700042853A1 (pl)
PL (1) PL3392328T3 (pl)
PT (1) PT3392328T (pl)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT202000001357A1 (it) 2020-01-24 2021-07-24 Itelyum Regeneration S P A Valorizzazione dei sottoprodotti di un processo di rigenerazione di olii usati
IT202000016126A1 (it) * 2020-07-03 2022-01-03 Itelyum Regeneration S P A Colonna di distillazione ausiliaria e suo uso

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT1255534B (it) * 1992-09-30 1995-11-09 Processo di riraffinazione di oli usati
US7261808B2 (en) * 2001-10-16 2007-08-28 Shell Oil Company Upgrading of pre-processed used oils
US9023755B2 (en) * 2012-12-18 2015-05-05 Cabot Corporation Siloxane removal from gases using lignite-enhanced activated carbons and adsorbent media used therefor
ITUB20151298A1 (it) * 2015-05-28 2016-11-28 Itelyum Regeneration S R L Procedimento di rigenerazione di olii usati

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

Also Published As

Publication number Publication date
EP3392328A1 (en) 2018-10-24
IT201700042853A1 (it) 2018-10-19
PT3392328T (pt) 2019-12-19
PL3392328T3 (pl) 2020-06-15
ES2753275T3 (es) 2020-04-07

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