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EP0835298B1 - Procede de raffinage d'huiles usagees par traitement alcalin - Google Patents

Procede de raffinage d'huiles usagees par traitement alcalin Download PDF

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Publication number
EP0835298B1
EP0835298B1 EP96924004A EP96924004A EP0835298B1 EP 0835298 B1 EP0835298 B1 EP 0835298B1 EP 96924004 A EP96924004 A EP 96924004A EP 96924004 A EP96924004 A EP 96924004A EP 0835298 B1 EP0835298 B1 EP 0835298B1
Authority
EP
European Patent Office
Prior art keywords
process according
water
approximately
alkaline agent
temperature
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.)
Expired - Lifetime
Application number
EP96924004A
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German (de)
English (en)
French (fr)
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EP0835298A1 (fr
Inventor
Bernard Chavet
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Individual
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Individual
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Publication of EP0835298A1 publication Critical patent/EP0835298A1/fr
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Expired - Lifetime legal-status Critical Current

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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
    • 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
    • C10M175/02—Working-up used lubricants to recover useful products ; Cleaning mineral-oil based

Definitions

  • the present invention relates to a process for refining used oils allowing refined oils to be reused, in particular as base oil, as fuel, or in an oil refinery.
  • the expression used oils means an oil or a mixture of oils in variable proportions, of various origins notably industrial applications.
  • oils intended for industrial uses or for engines contain various additives intended to give them specific properties required for the intended applications.
  • additives are either organic (so-called additives “ashless”) or organometallic. In all cases they are characterized, besides their specific function (such as anti-corrosion, anti-wear, antioxidant, dispersant ...) by a very good solubility in base oils (hydrocarbons with boiling points higher than 350 ° C), thermal stability as high as possible and finally volatility as low as possible.
  • Oils after use or used oils contain as impurities of such additives, either intact or in the form of decomposition products as well as sediment (wear particles from moving metal parts, air dust, carbon, etc.) and hydrocarbons not present in the original oils and which are undesirable.
  • These are petrol and diesel fractions, oxidation products (such as organic acids) and pyrolysis products. The presence of these different impurities makes refining used oils particularly difficult.
  • the phosphorus and silicon contents have been measured by plasma, the chlorine contents either by X-ray fluorescence (above 50 mg / kg) either by coulometry (below 50 mg / kg), the acid number was determined according to the French standard NFT 60112, the viscosity was measured at 40 ° C according to the method NFT 60100, color was measured according to ASTM D 1500 method, odor was sensory measured by the experimenter and the saponification index was measured by potentiometry.
  • oils thus pretreated they can be refined according to various processes in particular by catalytic hydrogenation at high pressure, or by treatment with concentrated sulfuric acid, by treatment with an activated earth or by the combination of these last two treatments and in some cases by distillation after one of these treatments.
  • the method according to the invention has in particular the advantage of being very flexible insofar as it can be adapted, as regards its characteristics, to the quality required of finished products.
  • the method according to the invention can be implemented following one or more preliminary, physical and / or chemical treatment processes, and / or upstream of one or more refining processes, such as those mentioned above.
  • the distillation stage (a) is firstly carried out at atmospheric pressure, at a temperature of about 130 to 180 ° C, to remove water and recover a fraction of gasoline.
  • the distillation is then continued, under a pressure of about 650 to 12,000 Pa and at a temperature of around 240 to 345 ° C, to recover a small fraction of diesel then a large fraction, greater than 60% of the used waste oil.
  • the whole distillate can be subjected to the subsequent step, preferably used according to the invention, the only significant fraction of the distillate.
  • This pre-distillation step is particularly important because it eliminates almost all tar.
  • the alkaline agent used in step (b) of the process is either sodium hydroxide or potash but never a mixture of soda and potash.
  • potash Preferably, according to the invention, potash.
  • the pH of the reaction medium is greater than 8 and preferably between 9.5 and 13.
  • the concentration of the alkaline agent in aqueous solution is preferably between 50 and 96% by weight relative to the weight of the aqueous solution.
  • the aqueous solution of alkaline agent is in the form of eutectic potash / water (86.7 / 13.3).
  • the aqueous solution of alkaline agent is prepared beforehand and is then added with continuous stirring to the distillate resulting from step (a). It can be “solid” at the ambient temperature, as is particularly the case for the potash / water eutectic (86.7 / 13.3), the use of which constitutes a particularly preferred embodiment. In this in this case, the "solid" solution becomes fluid at the reaction temperature.
  • the alcoholic solution used is preferably such that the ratio molar of said solvent to said alkaline agent is between 2 and 20, and more particularly between 2.5 and 5.
  • an amount is used alcohol or a mixture of alcohol sufficient to ensure in the reaction medium alkaline agent concentration close to saturation.
  • the monoalcohol or the polyalcohol preferably contains from 2 to 8 atoms of carbon, and more particularly from 2 to 5 carbon atoms.
  • ethanol n-propanol, isopropanol, n-butanol, sec-butanol, tert-butanol, isobutanol, pentanols, hexanols and octanols.
  • preferred polyalcohols according to the invention may include ethylene glycol, di- and tri-ethylene glycol. According to the invention, it is preferred to use alcohols with a boiling point below the initial boiling point of the distillate and / or having a high solubility in water because their subsequent elimination by distillation or washing with water is easier
  • the reaction medium is preferably prepared either by dissolving the alkaline agent in alcohol, then introduction into the distillate, either by hot mixing of distillate and alcohol then addition of the alkaline agent in the form of solid tablets.
  • step (b) of the method according to the invention when an alcohol or a mixture of alcohols is used as solvent, the treatment of the distillate with the alkaline agent is carried out at the reflux of the alcohol or of the mixture of alcohols provided, however, that there is no risk of loss by evaporation.
  • step (b) of the process according to the invention when operating at high temperature, and in particular when the solvent comprises an alcohol with a boiling point below the reaction temperature chosen, the distillate is treated with the alkaline agent at a pressure of approximately 10 5 to 50 x 10 5 Pa, preferably at a pressure of 10 5 to 25 x 10 5 Pa, in order to avoid losses by evaporation.
  • At the end of the alkaline treatment at least one washing of the medium is carried out reaction using approximately 1 to 15% of water at a temperature between room temperature and around 100 ° C.
  • the water washing operation or step (c) of the process according to the invention makes it possible to remove the excess of alkaline agent, possibly the alcohol if this was used as a solvent as well as all the soluble products from contaminants and generated by alkaline treatment.
  • the step of washing with water is carried out in a single operation, the latter is generally carried out using approximately 10% water at a temperature of approximately 100 ° C.
  • the step of washing is carried out in two separate operations.
  • the first is to treat the environment reaction obtained after step (b) with an amount of water of about 1 to 10% and at a temperature as low as possible, between 20 and 90 ° C.
  • the second is, after decanting, treating the reaction medium again with an amount of water included between 1 and 10% and at a temperature as high as possible and at least equal to that of the first operation.
  • the temperature should preferably be the as low as possible in order to minimize the hydrolysis phenomena but sufficient to lower the viscosity of the oily reaction medium of step (b) and guarantee a speed of sufficient settling.
  • the temperature must be the as high as possible to ensure good removal of the residual alkaline agent.
  • the total amount of water used according to this particular form of achievement is preferably between 5 and 15%.
  • the second washing operation can be carried out using a weak aqueous solution acid for example by means of hydrochloric acid 0.1 to 1 N.
  • distillation step (d) consisting initially of a distillation at atmospheric pressure and at a temperature of about 70 to 270 ° C, to remove the rest solvent, then at a pressure of around 1350 to 650 Pa and at a temperature about 210 to 375 ° C in order to obtain a refined oil and a residue which represents less 5% of the initial charge.
  • step (c) of washing with water the oily phase can be followed by at least one treatment of said oily phase with high pressure catalytic hydrogenation by contact with a sulfonating agent and / or by contacting with activated carbon or an activated earth.
  • the sulfonating agent is chosen from concentrated sulfuric acid and chlorosulfonic acid.
  • the activated earth is preferably a mineral earth of the silico-aluminate type activated by acid treatment.
  • this treatment is preferably followed by neutralization of the oily phase, by example by adding the washing water from step (c) and, preferably, by adding of ammonia.
  • the refined oil or the base oil obtained by the process according to the invention has excellent physical and chemical properties. She is practically odorless, weak in color and has very low chlorine contents, but also in phosphorus and silicon.
  • the main characteristics of the refined oils obtained by the process according to the invention are as follows: Chlorine content (mg / kg) ⁇ 35 Phosphorus content (mg / kg) ⁇ 5 Silicon content (mg / kg) ⁇ 5 Color (ASTM D 1500) ⁇ 3 Odor (sensory measurement) Very weak Water content (% by weight) ⁇ 10 -2 Sediments (% by weight) Absence Viscosity at 40 ° C (mm 2 / s) ⁇ 85 Acid number (IA; mgKOH / g) ⁇ 0.05 Saponification index (IS; mgKOH / g) ⁇ 0.20
  • the method of treatment according to the invention is particularly effective in reducing the main contaminants of used oils.
  • Fraction Pressure Temperature (° C) Proportion (% by weight) 1 1.013 x 10 5 130/180 7.5% (water + petrol) 2 5300-10700 240/285 9% (diesel) 3 650-2000 285/345 65%
  • the distillation residue represented approximately 18.5% and was mainly made up of tars.
  • the fraction representing 65% had the following characteristics: Chlorine content (mg / kg) 60 Phosphorus content (mg / kg) 27 Silicon content (mg / kg) 9 Color (ASTM D 1500) 6.5 Odor (sensory measurement) Very strong Water content (mg / kg) ⁇ 80 Sediments (% by weight) Absence Viscosity at 40 ° C (mm 2 / s) 31.24 Acid number (IA; mgKOH / g) 0.26 Saponification index (IS; mgKOH / g) 1.30
  • a part of the distillate fraction representing approximately 65% was treated under the conditions given in Table V below using an aqueous potassium hydroxide solution at 50% by weight relative to the weight of the solution, at a temperature of 300 ° C and under a pressure of 14 x 10 5 Pa and another part of this distillate using the potash / water eutectic (86.7 / 13.3), at a temperature of 220 ° C and at a pressure of 10 5 Pa.
  • the reaction medium was washed several times with water brought to a temperature of approximately 90 ° C. in order to remove the excess of alkaline agent and the different soluble products from alkaline treatment.
  • the characteristics of the refined oils obtained are also given in Table V. As can be seen from these two processes by alkaline treatment lead to a refined oil having identical characteristics as to the decrease in phosphorus, silicon and chlorine contents.
  • the pure potash to be used for reach the result is 7.2% or about 45 times the stoichiometry (IA + IS) if we uses a 50% and 0.47% aqueous solution of potash, or about three times the stoichiometry if the potash / water eutectic is used.
  • step (b) of the alkaline treatment was used of the process according to the invention at temperatures varying between 175 and 300 ° C for a duration from 10 to 60 minutes with n-octanol under the conditions indicated in Table VI below.
  • the amount of alkaline agent used was in all cases at least equal to twice the stoichiometry (IA + IS) and all the tests according to these examples were carried out under atmospheric pressure with the exception of examples 10 and 11 which were carried out under a pressure of 10 ⁇ 10 5 Pa.
  • the first half resulting from the treatment with 2% dry potash was divided into two equal parts.
  • washing in two operations leads to oils with a markedly improved color which is a result particularly unexpected.

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)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Fats And Perfumes (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Lubricants (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
EP96924004A 1995-06-22 1996-06-21 Procede de raffinage d'huiles usagees par traitement alcalin Expired - Lifetime EP0835298B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9507484 1995-06-22
FR9507484A FR2735785B1 (fr) 1995-06-22 1995-06-22 Procede de raffinage d'huiles usagees par traitement alcalin
PCT/FR1996/000974 WO1997000928A1 (fr) 1995-06-22 1996-06-21 Procede de raffinage d'huiles usagees par traitement alcalin

Publications (2)

Publication Number Publication Date
EP0835298A1 EP0835298A1 (fr) 1998-04-15
EP0835298B1 true EP0835298B1 (fr) 2001-05-23

Family

ID=9480271

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96924004A Expired - Lifetime EP0835298B1 (fr) 1995-06-22 1996-06-21 Procede de raffinage d'huiles usagees par traitement alcalin

Country Status (10)

Country Link
US (1) US6072065A (no)
EP (1) EP0835298B1 (no)
AT (1) ATE201438T1 (no)
CA (1) CA2222704A1 (no)
DE (1) DE69612978T2 (no)
DK (1) DK0835298T3 (no)
ES (1) ES2125208T3 (no)
FR (1) FR2735785B1 (no)
NO (1) NO976008L (no)
WO (1) WO1997000928A1 (no)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2766477B1 (fr) * 1997-07-22 1999-09-24 Bernard Chavet Procede de traitement d'une eau usee alcaline
US6007701A (en) * 1999-02-16 1999-12-28 Miami University Method of removing contaminants from used oil
US6238551B1 (en) * 1999-02-16 2001-05-29 Miami University Method of removing contaminants from petroleum distillates
FR2795421B1 (fr) * 1999-06-23 2001-10-05 Richard Deutsch Procede de decontamination des huiles minerales semi synthetiques et synthetiques usagees
CA2432993A1 (en) * 2002-07-08 2004-01-08 Infineum International Limited Molybdenum-sulfur additives
EP1382659B1 (en) * 2002-07-08 2007-01-24 Infineum International Limited Process for making molybdenum-sulfur additives containing little unreacted sulfur and additives obtained by the process
ES2199697B1 (es) * 2003-09-23 2005-02-01 Sener Grupo De Ingenieria, S.A. Procedimiento para regenerar aceites usados por desmetalizacion y destilacion.
FR2961521B1 (fr) * 2010-06-22 2013-07-12 Conception D Equipements Pour L Environnement Et L Ind Soc D Procede de purification d'une charge hydrocarbonee usagee
FR3039162B1 (fr) * 2015-07-20 2020-02-28 Societe De Conception D'equipements Pour L'environnement Et L'industrie Purification d'huile et preparation d'additif anti-ornierage
FI128069B2 (en) 2018-07-20 2024-04-24 Neste Oyj Purification of recycled and renewable organic material
FI128115B2 (en) 2018-07-20 2024-08-20 Neste Oyj Purification of recycled and renewable organic material
FI128121B (en) 2018-07-20 2019-10-15 Neste Oyj Production of hydrocarbons from recycled or renewable organic material
FI128174B (en) 2018-07-20 2019-11-29 Neste Oyj Purification of recycled and renewable organic material
FI128911B2 (en) 2018-07-20 2025-05-27 Neste Oyj Cleaning of recycled and renewable organic material
FR3130826A1 (fr) * 2021-12-21 2023-06-23 Totalenergies Marketing Services Méthode de purification d’huiles lubrifiantes au moins en partie re-raffinées

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1470599B2 (de) * 1963-10-23 1971-07-15 Mitsubishi Jukogyo K.K., Tokio Verfahren zur kontinuierlichen entfernung von verunreinigung aus schmieroel und vorrichtung zur durchfuehrung des ver fahrens
AT262479B (de) * 1965-10-21 1968-06-10 Oemv Ag Verfahren zur Aufarbeitung von gebrauchten Schmierölen
US3625881A (en) * 1970-08-31 1971-12-07 Berks Associates Inc Crank case oil refining
US3793184A (en) * 1971-09-09 1974-02-19 Dow Chemical Co Reconditioning oil used in cold working metal
DE2508713C3 (de) * 1975-02-28 1979-04-12 Adolf Schmids Erben Ag, Bern Verfahren zur Aufarbeitung von gebrauchtem Mineralöl
CA1181771A (en) * 1982-07-27 1985-01-29 Ontario Hydro Process for dehalogenation of organic halides
CH657867A5 (de) * 1983-09-21 1986-09-30 Buss Ag Verfahren zur wiederaufbereitung von altoel und destillations-vorrichtung zur durchfuehrung des verfahrens.
CA2068905C (en) * 1992-05-19 1997-07-22 Terry A. Wilson Waste lubricating oil pretreatment process

Also Published As

Publication number Publication date
DE69612978D1 (de) 2001-06-28
US6072065A (en) 2000-06-06
FR2735785A1 (fr) 1996-12-27
ES2125208T3 (es) 2001-09-01
NO976008D0 (no) 1997-12-19
EP0835298A1 (fr) 1998-04-15
WO1997000928A1 (fr) 1997-01-09
DK0835298T3 (da) 2001-08-27
ES2125208T1 (es) 1999-03-01
NO976008L (no) 1998-02-23
CA2222704A1 (fr) 1997-01-09
ATE201438T1 (de) 2001-06-15
DE69612978T2 (de) 2001-12-20
FR2735785B1 (fr) 1997-08-08

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