EP4534635B1 - Verfahren zur herstellung von bioschmiermitteln aus abfallmaterialien - Google Patents

Verfahren zur herstellung von bioschmiermitteln aus abfallmaterialien

Info

Publication number
EP4534635B1
EP4534635B1 EP23425054.6A EP23425054A EP4534635B1 EP 4534635 B1 EP4534635 B1 EP 4534635B1 EP 23425054 A EP23425054 A EP 23425054A EP 4534635 B1 EP4534635 B1 EP 4534635B1
Authority
EP
European Patent Office
Prior art keywords
waste
lubricants
reactor
outlet
biolubricants
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
EP23425054.6A
Other languages
English (en)
French (fr)
Other versions
EP4534635C0 (de
EP4534635A1 (de
Inventor
Giuseppe Magnone
Francesco NEGRI
Oscar PELIS
Alessandro QUAGLIA
Aldo ROLDI
Gianluca FUGAZZA
Marco CODOGNOLA
Francesco Gallo
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.)
Itelyum Regeneration SpA
Original Assignee
Itelyum Regeneration SpA
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 Itelyum Regeneration SpA filed Critical Itelyum Regeneration SpA
Priority to EP23425054.6A priority Critical patent/EP4534635B1/de
Priority to PCT/IB2024/059213 priority patent/WO2025074190A1/en
Publication of EP4534635A1 publication Critical patent/EP4534635A1/de
Application granted granted Critical
Publication of EP4534635B1 publication Critical patent/EP4534635B1/de
Publication of EP4534635C0 publication Critical patent/EP4534635C0/de
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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
    • C10M175/0016—Working-up used lubricants to recover useful products ; Cleaning with the use of chemical agents
    • 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
    • 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
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/40—Fatty vegetable or animal oils
    • C10M2207/401—Fatty vegetable or animal oils used as base material

Definitions

  • wastes were hardly a problem before the mass production since objects used to be used and repaired until they failed or broke down. In this way, wasted products did not pollute air, water, or soil, since there was not a critical mass for that. This is no longer the situation, now.
  • a process which allows to reuse the biological fraction of waste lubricants on one hand and waste vegetable oils, like UCO and RUCO, and biolubricants on the other hand, comprising a series of treatments leading the two groups of waste oils to be transformed into the same product, which is then mixed, hydrolysed and treated, in order to get biolubricants.
  • the treatments that waste vegetable oils and biolubricants undergo include centrifugation.
  • a centrifugation takes place in more than one step, most preferably in three steps.
  • the first one is carried out on the waste vegetable oils as such, preferably after heating and stirring, so removing wastewater and solids;
  • the second step is carried out on the liquids leaving the first centrifugation step; preferably, before such second centrifugation step, the liquid is washed with distilled water.
  • the second centrifugation step allows to remove wastewater and rubbers which are soluble in water.
  • the third step takes place on the liquid coming from the second centrifugation step.
  • the liquid is reacted with H 3 PO 4 .
  • wastewater coming from the centrifugation steps are neutralised with a strong base.
  • the third centrifugation step allows to remove wastewater and rubbers which are not soluble in water.
  • the liquids coming from the previous two treatments are mixed together, before undergoing further process steps.
  • the oily phase is dehydrated.
  • the dehydrated oily phase undergoes a purification step.
  • a purification step includes distillation.
  • such a distillation takes place in a plate distillation column.
  • this distillation allows to separate the oily phase from bitumen, which is stored for sale, and ZnO, which can be recovered and employed.
  • the distillation residue, containing bitumen and ZnO undergoes an enhancement process.
  • such enhancement includes dissolving this residue in an apolar solvent, filtering off and/or centrifuging the product of such a dissolution, obtaining a solid and a liquid phase, wherein the solid phase is directly used as hydrolysis catalyst and the liquid phase undergoes a removal of the solvent by distillation, which is recycled for the dissolution of further residue, obtaining a paste which is used as raw material for dyes.
  • the oily phase undergoes esterification with alcohols.
  • esterification is carried out in the presence of acids as catalyst.
  • the products of the esterification step are purified, preferably by distillation. The residue can be partially recycled to the esterification step.
  • the other fraction coming from the centrifugal separator 39 is brought, through a pipe 44 to a tank 45.
  • the contents of the tank 45 can be brought, through a pipe 46, to the reactor 21.
  • the reactor 21 is fed also by two further inlets, 47 and 48. Therefore, the reactor 21 is fed by pipes 22, 46, 47 and 48.
  • Another outlet 67 leaves the reactor 21 and feeds a tank 68.
  • the contents of the tank 68 can be fed through a pipe 69 to a reactor 70, preferably stirred and heated, in order to ensure the best reaction conditions.
  • the reactor 70 is fed also by inlets 71 and 72.
  • the inlet 1 leads to a pre-flash column 3, wherein a pre-flash step 76 takes place.
  • the pre-flash step 76 is carried out at a temperature of 100 to 200 °C, preferably at 130-150 °C, in order to balance a low energy consumption and a good removal of water from the oils.
  • Water is removed through the outlet 77, while the oils to be regenerated go to a subsequent step 78, wherein fatty acids, coming from the oils to be regenerated are recovered.
  • This step 78 takes place in the plant units bearing the numerals 4-7 and 9-20.
  • the oils are contained in the tank 9, until the next process is started. At this point, the oils are heated in the heat exchanger 11 up to a temperature ranging from 50 to 110 °C, preferably from 70 to 90 °C, in order to ensure the best reaction conditions.
  • the biolubricants are then fed to the reactor 12, where they are added of sulfuric acid from the feed 13.
  • Sulfuric acid is added from the feed 13 at a concentration of 30 to 98 wt.% and the addition is such that the solution added to the oils in the reactor 12 ranges from 1 to 20 wt.%, preferably from 5 to 10 wt.%; at such a concentration, the hydrolysis and the conversion of soaps into acids is complete.
  • the product exits through the outlet 15 and is washed with water coming from the inlet 17 in the reactor 16.
  • the wastewater is downloaded through the pipe 18, while the product is fed to the tank 20 through the pipe 19.
  • Wastewater and solids, containing rubbers which are not water soluble, are removed through the pipe 34, while the matters to be regenerated are fed to the reactor 36, where 1 to 20 wt.%, preferably 5 to 10 wt.% of an aqueous solution of H 3 PO 4 , generally at a concentration of 30 to 80 wt.%, is added by the pipe 37.
  • the reaction product is fed to the last centrifugal separator 39 at a temperature ranging from 50 to 110°C, preferably from 70 to 90 °C and with a stirring of 2,000 to 10,000 rpm. Wastewater and solids are removed through the outlet 40 and the matter to continue the treatment is fed, through a pipe 44 to the tank 45, completing the step 79.
  • Wastewater and solids fed to the reactor 28 are acid, so that they are neutralised with a strong base, like CaOH, NH 3 or NaOH; wastewater coming from the outlet 42 is sent to the water purification and phosphate-based fertilisers, which are a valuable co-product, are then recovered from the outlet 43.
  • a strong base like CaOH, NH 3 or NaOH
  • Matters coming from the preliminary steps are contained in tanks 20 and 45. They are sent from the said tanks 20 and 45 to the reactor 21, where they are combined and where a hydrolysis step 80 takes place. They are added with ZnO which acts as a catalyst (from the inlet 47) and water (from the inlet 48). Preferably, ZnO is added at 1 to 5 wt.%, preferably at 2 wt.% and water is added in order to be 20 to 40 wt.%, preferably 30 wt.%.
  • the hydrolysis takes preferably place at 150-250 °C and 10-20 bar for 6 to 18 hours.
  • the products of the hydrolysis step 80 are an aqueous phase, containing raw glycerine, and an oily phase, mainly containing fatty acids. Such product of hydrolysis is splitted into two flows, one bringing glycerine to be purified, which is another valuable co-product, and the other one is purified and esterified.
  • the head fraction is sent to the water treatment facility and the tail in the outlet 57 is then sent to the column 61, where temperature is 250-350 °C at the bottom and 30 to 60 °C at the head and pressure is 0.0130-0.0150 at the bottom and 0.002 to 0.005 at the head, from where wastewater exits from the outlet 62, glycerine from the outlet 63 and is stored in the tank 65 and bitumen through the outlet 64 and is stored in the tank 66, both for delivery and subsequent sale.
  • the other part of the product is temporarily stored in the tank 68, after dehydration -which can take place under stirring at 130-200 °C for 1-2 hours- from where, after a conventional purification step 82 -preferably distillation-, it passes to an esterification step 83.
  • a distillation is normally carried out at a pressure of 6.6x10 -3 to 0.0020 bar and is normally stopped when the boiling point, referred to atmospheric pressure, is 405°C, normally with a residence time of 3-6 hours.
  • the distillation residues contain mainly bitumen and ZnO. ZnO is recovered and can easily be reused.
  • the bitumen can be added to the other bitumen fractions obtained.
  • the esterification takes place batchwise in the reactor 70, where the acids arrive through the pipe 69 from the tank 68, where (vide infra) also a recycle is added. Also some weak acids, like pelargonic or adipic acids, are added as co-reactants from the inlet 72 and alcohols, like n-decanol or trimethylolpropane (TMP) are added in a stoichiometric amount through the inlet 71. Wastewater leaves the plant through the outlet 73 and goes to the water treatment plant, while raw biolubricants leave through the outlet 74 to a purification step 84 and subsequently to the tank 75, where they are stored for the delivery and sale.
  • weak acids like pelargonic or adipic acids
  • alcohols like n-decanol or trimethylolpropane (TMP)
  • a recycle of fatty acids taken from wastewater in 73 takes place through a pipe 85 to the tank 68.
  • the fatty acids are distilled at 6.6x10 -3 to 0.0020 bar, stopping the distillation as soon as the flow rate dramatically drops, normally after 3 to 6 hours.
  • the bitumen coming from the distillation residue of the step 82 can undergo a process for the enhancement of the organic molecules therein contained.
  • this residue instead of mixing this residue to the other bitumen obtained in other steps of this process or even in other processes, taking place in the same industrial site, this residue is dissolved in an apolar solvent, like a saturated, linear hydrocarbon, such as n-pentane, n-hexane, n-heptane, n-octane, n-nonane, n-decane.
  • the solution obtained is stirred for 1 to 4 hours.
  • the solution is then filtered off and/or centrifuged and two phases are obtained, one being solid and the other being liquid.
  • the solid part contains ZnO and can directly be used as catalyst in the reactor 21 without any further purification, in the hydrolysis step 80, so reducing the consumption of fresh catalyst, with a cost saving.
  • the solvent can be removed by distillation and recycled to the first step of this part of the process and the paste remaining can be used as raw material for the production of dyes.
  • the present invention allows to combine two processes for the regeneration of different kind of oils -namely lubricants on one hand and UCO and RUCO on the other hand-, providing a useful product and avoiding wastes which are not wastewater, with energy costs limited and it is therefore surely part of the so called circular economy.

Landscapes

  • 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)

Claims (10)

  1. Verfahren zur Herstellung von Bioschmierstoffen aus Abfallstoffen, wobei es sich bei den Abfallstoffen um Bioschmierstoffabfälle, gebrauchte Speiseöle mit der Bezeichnung UCO, regenerierte gebrauchte Speiseöle mit der Bezeichnung RUCO und eine biologische Fraktion von Schmierstoffabfällen handelt, wobei zwei Leitungen (22, 46) für eine nachfolgende Reaktion (80) nach zwei getrennten Vorbehandlungen kombiniert werden, wobei die erste Leitung (46) Bioschmierstoffabfälle, UCO und RUCO, die verarbeitet wurden, bringt und die zweite Leitung (22) eine biologische Fraktion von Schmierstoffen, die von Schmierstoffabfällen getrennt sind, bringt, wobei die biologische Fraktion von Schmierstoffabfällen durch einen Vorentspannungsschritt (76) von Schmierstoffabfällen und einen nachfolgenden Schritt in einem Dekanter (5), aus dem diese biologische Fraktion aus dem Sumpf entnommen wird, geführt wird und wobei das Hydrolyseprodukt in zwei Ströme aufgeteilt wird, eine wässrige Phase, die rohes Glycerin enthält, und eine ölige Phase, die hauptsächlich Fettsäuren enthält, dadurch gekennzeichnet, dass Bitumen, das aus dem Destillationsrückstand eines Reinigungsschritts (82) von Produkt, das aus einer Bodendestillationskolonne (61) kommt, stammt, einem Prozess zur Anreicherung der organischen Moleküle unterzogen wird, wobei dieser Rückstand in einem apolaren Lösungsmittel gelöst wird, die erhaltene Lösung gerührt wird, dann abfiltriert und/oder zentrifugiert wird, um Katalysator und einen Rohstoff für Farbstoffe zu trennen.
  2. Verfahren nach Anspruch 1), dadurch gekennzeichnet, dass die Vorbehandlung (79) von UCO und RUCO aus einem Zentrifugationsschritt besteht, der zwei Fraktionen trennt: eine flüssige und eine, die Abwasser und Feststoffe enthält.
  3. Verfahren nach Anspruch 2), dadurch gekennzeichnet, dass mehrere Zentrifugationsstufen (79) bereitgestellt werden.
  4. Verfahren nach Anspruch 3), dadurch gekennzeichnet, dass zwischen zwei Zentrifugationsstufen destilliertes Wasser und/oder eine wässrige Lösung von H3PO4 zu der flüssigen Fraktion in Behandlung hinzugefügt werden.
  5. Verfahren nach einem der Ansprüche 2) bis 4), dadurch gekennzeichnet, dass die Fraktion, die Abwasser und Feststoffe enthält, mit einer starken Base, wie CaOH, NH3 oder NaOH, neutralisiert wird.
  6. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die biologische Fraktion, die aus dem Boden des Dekanters (5) entnommen wird, mit Schwefelsäure umgesetzt wird.
  7. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass Flüssigkeiten, die den Vorbehandlungen unterzogen wurden, in einem Reaktor (21) kombiniert werden, wo eine Hydrolysereaktion (80) stattfindet.
  8. Verfahren nach Anspruch 7), dadurch gekennzeichnet, dass die Stoffe, die in den Reaktor (21) eintreten, mit ZnO (aus dem Einlass 47) und Wasser (aus dem Einlass 48) bei 150-250 °C und 10-20 bar hinzugefügt werden.
  9. Verfahren nach Anspruch 8), dadurch gekennzeichnet, dass ZnO mit 1 bis 5 Gew.-% hinzugefügt wird und Wasser hinzugefügt wird, um bei 20 bis 40 Gew.-% zu sein.
  10. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass ein oder mehrere Schritte chargenweise durchgeführt werden.
EP23425054.6A 2023-10-02 2023-10-02 Verfahren zur herstellung von bioschmiermitteln aus abfallmaterialien Active EP4534635B1 (de)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP23425054.6A EP4534635B1 (de) 2023-10-02 2023-10-02 Verfahren zur herstellung von bioschmiermitteln aus abfallmaterialien
PCT/IB2024/059213 WO2025074190A1 (en) 2023-10-02 2024-09-23 Process for the production of biolubricants from waste materials

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP23425054.6A EP4534635B1 (de) 2023-10-02 2023-10-02 Verfahren zur herstellung von bioschmiermitteln aus abfallmaterialien

Publications (3)

Publication Number Publication Date
EP4534635A1 EP4534635A1 (de) 2025-04-09
EP4534635B1 true EP4534635B1 (de) 2025-12-17
EP4534635C0 EP4534635C0 (de) 2025-12-17

Family

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Country Status (2)

Country Link
EP (1) EP4534635B1 (de)
WO (1) WO2025074190A1 (de)

Family Cites Families (3)

* 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
GB2436836A (en) * 2006-03-31 2007-10-10 Greenergy Biofuels Ltd Removal of free fatty acids from used cooking oil prior to biodiesel production
EP4457324B1 (de) * 2021-12-30 2026-02-04 Isuschem s.r.l. Verfahren zur herstellung von bioschmierölen

Also Published As

Publication number Publication date
WO2025074190A1 (en) 2025-04-10
EP4534635C0 (de) 2025-12-17
EP4534635A1 (de) 2025-04-09

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