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

Definitions

• the present invention relates to a process and an installation for regenerating high-performance used lubricating oils.
• the invention relates to a process for regenerating used lubricating oils having a low content of fuel oil, fatty acids and chlorinated products, in which the used lubricating oils are subjected to the following successive treatment steps in order: ) selection of used oils suitable for treatment; b) adding a first quantity of a strong base in aqueous solution; c) heating the mixture to a temperature between 120 and 250 ° C; d) adding a second quantity of the strong base in aqueous solution, the first and the second quantity of strong base in aqueous solution representing together from 0.5 to 3% of pure bases by mass of used lubricating oils; e) dehydration and extraction of light hydrocarbons; f) extraction and recovery of gas oil (stripping); g) extraction of impurities.
• a complementary addition of a strong base in aqueous solution due to 0.1 to 1% of pure bases by mass of lubricating oils is carried out after step e).
• the invention can also have the characteristics below considered in isolation or in all their technically possible combinations:
• the stripped oil is freed of its impurities (residues) in a vacuum column provided with a reboiling system, then subjected to a stage oxidation before the additional addition of strong bases, then fractionated, -
• the elimination of impurities is obtained by vacuum distillation ensuring the separation into lubricating base oils on the one hand, and in a residue concentrating all the impurities on the other hand.
• the amount of strong bases in aqueous solution provided may be between 0.5 to 3% of pure bases by mass of used lubricating oils.
• This addition can be made totally or partially cold or hot.
• the heating temperature of the used oils to be regenerated between 120 and 250 ° C. is a temperature at which the addition of the hot base is carried out in whole or in part.
• FIG. 1 is a schematic representation of a process and an installation for regenerating used lubricating oils of the prior art
• FIG. 2 is a schematic representation of a process and a regeneration system of used lubricating oils in a first embodiment of invention 1 •;
• FIG. 3 is a schematic representation of a process and an installation for regenerating used lubricating oils according to a second embodiment of the invention
• FIG. 4 is a schematic representation of a process and an installation for regenerating used lubricating oils according to a third embodiment of the invention.
• the used oils collected can have various origins. It can be, for example, engine oil, gear oil, hydraulic oil, turbine oil, etc. When these oils arrive in the regeneration unit, their suitability for processing is checked.
• the regeneration process of the invention aims to eliminate light components, such as petrol, diesel and water, it also allows the elimination of degradation products from oil and additives, but does not make it possible to eliminate certain components as heavy as the oils themselves and having different physical properties. It could be, for example, fuel whose elimination or treatment could only be obtained by a complete refining process.
• regenerability tests are as follows: - The "Chlor test” makes it possible to detect the presence of chlorides. A copper wire dipped in used oil is presented to the flame. A greenish flame indicates the presence of chlorides.
• the "Drop test” detects the presence of fuel. A drop of oil is deposited on a chromatographic paper. A concentric spot with a yellowish halo indicates the presence of fuel.
• the "Fat test” detects the presence of fatty acids in oils. 2 ml of used oil is heated in the presence of a soda tablet: when the oil freezes, after cooling, this means that fatty acids are present.
• PCB polychlorinated biphenyl
• waste oils collected 1 having successfully undergone all of the tests are combined in a tank 2. They are then mixed, either inside the tank 2, or during their extraction by conventional means not shown in the Figures .
• a base or a mixture of bases stored elsewhere in a tank 4a is provided and mixed by means 5a with the used oils at room temperature between 10 and 40 ° C.
• Heating means 3 bring the oils taken from the tank 2 and optionally mixed with the base, to a temperature between 120 and 250 ° C and preferably between 140 and 160 ° C.
• a base or a mixture of bases stored elsewhere in a tank 4b is supplied and mixed by means 5b with the heated waste oils.
• an amount of pure bases of between 0.5 and 3% by mass is added to the used oils.
• This rate as well as its distribution between the two cold and hot injection points, can be advantageously specified depending on the quality of the used oils and the nature of the base used.
• the base used is a strong base, preferably sodium or potassium hydroxide.
• a strong base preferably sodium or potassium hydroxide.
• Waste oils brought to a high temperature, added with strong base, feed a unit 6 for extraction of water and light hydrocarbons by expansion (flash).
• a unit 6 for extraction of water and light hydrocarbons by expansion the evaporation of water is produced by the sudden expansion of the mixture in a balloon.
• Water and light hydrocarbons are extracted and discharged to outlet 7.
• the remaining mixture is directed to a unit 8 for extracting gas oil (stripping). This elimination is carried out by distillation in a column.
• the gas oil 9 is then evacuated and the remaining mixture is led to a distillation column 10 allowing the fractionation of the mixture into sections of lubricating base oils 11, 12 and the separation of the residue 15 where all the impurities are concentrated.
• Base oils can be separated at different levels depending on the number of cuts desired.
• the distillation column 10 is a traditional column under vacuum which allows the dissociation and extraction of the residues which are directed to an accumulation tank 14.
• the residues 15 are then removed and are capable of being used, for example, as tar or bitumen for the construction of roads. They can also be used as fuel.
• the vacuum distillation column 10 is preferably associated with a column bottom exhaustion evaporator 13 making it possible to improve its efficiency.
• Part of the energy required to raise the temperature of the used oils before the flash preferably comes from the energy recovery carried out on the sections of lubricating base oils 11, 12 from the column outlet 10.
• the used oils are advantageously filtered during their recovery and when they leave the storage tank 2, so as to remove the solid particles which they may contain.
• Different pumps, not shown, ensure the circulation of the mixture and of the products extracted through the installation described.
• An addition of additional base solution is made in lower proportions than the initial additions, before the flash, the additional addition being in proportions of the order of 0.1 to 1% by mass of pure bases relative to the used lubricating oils. It can be carried out at different points of the installation corresponding in each case to an embodiment.
• This process makes it possible to ensure better stability of the regenerated base oils and to fluidize the impurities, which allows easier operation of the process.
• the oil temperature is then advantageously between 270 and 310 ° C.
• the addition of complementary base is carried out under the same concentration and temperature conditions as in the first embodiment, but after the gas oil extraction operation (stripping ).
• a base stored in a tank 18 is supplied and mixed by means 19 with the heated stripped oil directed towards the fractionation column.
• an evaporator 13 following the stripping operation of gas oil, an evaporator 13, preferably with thin layers, coupled to a vacuum column 10, makes it possible to eliminate most of the impurities.
• the oil obtained is then subjected to accelerated oxidation in a tank 22, before an additional quantity of pure bases is added to it.
• a base stored in a reservoir 23b is supplied and mixed with the oil by mixing means 24.
• the oil is then fractionated in the distillation column 20.
• the temperature of the oil during the addition of the base is advantageously between 200 and 300 ° C for an injection from the reservoir 23b just before column 20 and is between 120 and 200 ° C for an addition from of a reservoir 23a directly in the oxidation tank 22.
• the evaporator 13 is advantageously a thin film evaporator. It is also possible to use several evaporators successively.
• the residues 21 of column 20 are, depending on the efficiency of this column and the requirements imposed on the regenerated oils, either recirculated and injected at the inlet of column 10, or conveyed to the storage of the residues such as the residues 15 coming from the distillation column 10 and 1 • evaporator 13.
• This choice is a function of the concentration of residues 21 in lubricating oil. It is done regularly according to the requirements imposed on regenerated oils.
• sample 2 was obtained by a process according to the invention implemented according to one of Figures 2 and 3.
• Sample 3 was obtained by a process according to 1 invention implemented according to Figure 4 These samples are compared to sample 1 obtained with a single basic injection according to the prior art.
• samples 5 and 6 obtained according to the invention are to be compared with sample 4 obtained according to the prior art.

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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)
• Lubricants (AREA)

Applications Claiming Priority (3)

Publications (2)

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ID=9498674

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• 1996
  • 1996-12-13 FR FR9615380A patent/FR2757175B1/fr not_active Expired - Fee Related
• 1997
  • 1997-05-12 UA UA99063267A patent/UA59382C2/uk unknown
  • 1997-11-24 TN TNTNSN97189A patent/TNSN97189A1/fr unknown
  • 1997-12-05 HU HU0001433A patent/HU222544B1/hu active IP Right Grant
  • 1997-12-05 AT AT97950242T patent/ATE200302T1/de active
  • 1997-12-05 AU AU53269/98A patent/AU5326998A/en not_active Abandoned
  • 1997-12-05 WO PCT/FR1997/002224 patent/WO1998026031A1/fr not_active Ceased
  • 1997-12-05 CZ CZ0211899A patent/CZ300297B6/cs not_active IP Right Cessation
  • 1997-12-05 PL PL97334068A patent/PL186318B1/pl unknown
  • 1997-12-05 CA CA002274831A patent/CA2274831C/fr not_active Expired - Lifetime
  • 1997-12-05 ES ES97950242T patent/ES2156008T3/es not_active Expired - Lifetime
  • 1997-12-05 RU RU99115454/04A patent/RU2187544C2/ru active
  • 1997-12-05 DE DE69704500T patent/DE69704500T2/de not_active Expired - Lifetime
  • 1997-12-05 EP EP97950242A patent/EP0944696B1/de not_active Expired - Lifetime
  • 1997-12-05 PT PT97950242T patent/PT944696E/pt unknown
  • 1997-12-05 DK DK97950242T patent/DK0944696T3/da active
  • 1997-12-10 DZ DZ970219A patent/DZ2369A1/xx active
  • 1997-12-12 AR ARP970105867A patent/AR010353A1/es unknown
  • 1997-12-12 MA MA24900A patent/MA24424A1/fr unknown
• 1999
  • 1999-07-11 OA OA9900121A patent/OA11060A/fr unknown
  • 1999-07-13 BG BG103577A patent/BG64486B1/bg unknown
• 2001
  • 2001-06-19 GR GR20010400918T patent/GR3036074T3/el unknown

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