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WO1995008609A1 - Microfiltration d'huile usee - Google Patents

Microfiltration d'huile usee Download PDF

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Publication number
WO1995008609A1
WO1995008609A1 PCT/CA1994/000524 CA9400524W WO9508609A1 WO 1995008609 A1 WO1995008609 A1 WO 1995008609A1 CA 9400524 W CA9400524 W CA 9400524W WO 9508609 A1 WO9508609 A1 WO 9508609A1
Authority
WO
WIPO (PCT)
Prior art keywords
used oil
microfiltration
oil
permeate
flow
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.)
Ceased
Application number
PCT/CA1994/000524
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English (en)
Inventor
Piero D'amore
Siamak Mirmiran
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.)
Individual
Original Assignee
Individual
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 Individual filed Critical Individual
Priority to AU77361/94A priority Critical patent/AU7736194A/en
Publication of WO1995008609A1 publication Critical patent/WO1995008609A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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
    • C10M175/06—Working-up used lubricants to recover useful products ; Cleaning by ultrafiltration or osmosis

Definitions

  • Microfiltration refers to a membrane permeation filtration process where a membrane acts as a particle trapping sieve acting on a fluid which passes through it. Microfiltration is generally performed with pore sizes ranging form 0.1 to 0.5 microns.
  • the expression “USED OIL” refers to a fluid which is discarded, after having been used for lubricating purposes and the like, when degradation of the fluid has gradually made it unfit for its intended purpose. The degradation takes place more or less rapidly as impurities enter the fluid or as chemical and physical degradation occurs.
  • the following categories of fluids are generally covered by the expression “USED OIL”: lubricating oils (motor, turbine, gear and the like); hydraulic systems oils (including transmission oils); metal working oils (including cutting, wetting, milling, rolling, coating oils and the like); insulating or heat transfer oils; residuals oils (including oily liquids, water/oil emulsions, greases and organic solvents and oil mixtures). Used oils primarily contain hydrocarbons.
  • Used oils can also contain various additives and solvents along with physical and chemical impurities (for example solids such as dirt, metals and the like).
  • used oils are classified in most industrialized countries as constituting hazardous wastes.
  • the elaboration of systems for the efficient recycling of used oils such as lubricating oils is increasingly necessary in view of the important volume of such fluids which are discarded after having performed their useful function as, for example, in the case of motor vehicle engine oil. Consequently the proper disposal or recycling of used oils is of primary importance.
  • Used oils can be recycled or otherwise treated by various known methods. For example, some of the industrial used oils regeneration processes currently used in North America are as follow: acid/clay treatment; vacuum distillation/clay; vacuum distillation/hydrotreatment; chemical treatment/distillation/hydrotreatment.
  • Keim et al in U.S. Patent 5,049,258 propose a distillation followed by hydrocracking treatment to eliminate chlorinated contaminants found in some used oils.
  • used oil is initially heated to a temperature between 200 and 500 °C under a pressure of 0.1 to 50 bars and then fractionated to remove light fractions and water vapor. Afterwards, using polymeric ultrafiltration membranes, the oil is filtered at a temperature between 10 °C to 80 °C. This latter operating temperature is quite low and corresponds to the typically low resistance limits of the ultrafiltration membrane.
  • the obvious disadvantages of this process are its high energy consumption, the fragile nature of the ultrafiltration membrane, and the very low ultrafiltration temperatures dictated by the membrane resistance which slows and generally hampers the filtration process as the oil is increasingly viscous and its flow becomes less turbulent as its temperature is reduced.
  • Pat. No. 4,784,751 advocate the use of a coarse filter to eliminate solid impurities. The used oil is then heated to 180 °C to remove water and volatile fractions fraction.
  • a further object is to obtain by the process and method of the present invention a regenerated oil with a composition, viscosity, and color similar to that of fresh oil.
  • Still further objects are to obtain process improvements resulting in an increased yield in purified oil on a weight percent basis of the used oil.
  • Related objects are to reach improvements in the following areas: improved process control capabilities; obviating the need to evaporate light fractions; improved recuperation of metallic contaminants; increased quality and viscosity of the recycled oil; reduction of filtration membrane clogging; and increased viscosity of the by-product (retentate) of the recycling process.
  • the by-product of the recycling process which is essentially a concentration of contaminants present in the used oil feed can also be usefully recycled by known processes for diverse uses such as bitumen preparation or synthetic rubber manufacturing.
  • the system of the present invention is intended for use in a process for recycling used oils at yields reaching in excess of 90 percent of recycled oil per volume of used oils.
  • the system of the present invention comprises: a feedstock of used oil entering the system through a feed line, circulation pump means for pumping a flow of used oil at a pressure of at least 105 psi, heat exchange means for heating said flow of used oil at a temperature of 200 °C to 500 °C, at least one microfiltration unit containing a plurality of microfiltration membranes with pore sizes ranging from 0.1 and 0.5 microns for microfiltering said flow of used oil and separating therefrom a permeate of recycled oil and retaining a retentate of used oil for recirculation in the system, whereby during operation of the system, the flow of used oil upstream of the microfiltration means is controlled by monitoring temperature or pressure in the system to remain at a Reynolds number of at least 2300.
  • the present invention also discloses a method of recycling used oil using the system of the present invention and comprising the steps of :
  • the present invention using a microfiltration method yields oils essentially free of metallic impurities.
  • the microfiltration membrane acts as a particle sieve to retain these and other impurities in a retentate.
  • the retentate can also be further recycled by known processes to extract useful substances therefrom.
  • valves 36, 38, and 40 are open while valve 35 is closed to pass the used oil through the microfiltration unit 42 containing microfiltration membranes having pores sizes inferior to 0.5 micron, and preferably between 0.1 to 0.5 micron.
  • the filtrated oil (permeate) is routed toward holding tank 44.
  • the circulation loop flow of concentrated used oil is maintained at a Reynolds number of at least 2500 and preferably 3000. This is done by supplying further heat and pump pressure to the circulation loop. When the Reynolds number of the circulation loop flow drops to approximately 2500, the retentate is directed to the tank 46. This operation is automatically accomplished by an automatic signal received from a viscometer 48 on valve 36. In order to avoid heat loss, the system is properly insulated.
  • microfiltration unit designs could be used such as stack, cross-flow or bi-flow stack, and spiral module designs.
  • FIG 5 shows a two-stage cascading system.
  • the two-stage system is a cascade of two distinct systems (A and B) which are each essentially similar to the continuous mode system of FIG 2.
  • the difference between units A and B lies in the pore size of the microfiltration membranes. Since Unit B receives the permeate of Unit A and is equipped with finer microfiltration membranes to further remove contaminants that may still be present.
  • the used oil is injected into unit A by a gear pump 58, having a variable speed motor.
  • a variable speed centrifugal pump 60 maintains a pressure of 150 psi up-stream of the microfiltration unit 62.
  • the circulation rate is calculated depending on the viscosity of the oil in order to reach a Reynolds number preferably superior to 3000 corresponding to a sufficiently turbulent flow.
  • the heat exchanger 64 heats the used oil to a temperature superior ranging from 200 to 500 °C. To maintain a Reynolds number superior to 3000 during the use of the system, the operating temperature will be constantly adjusted as a function of the viscosity of the used oil entering the system.
  • the heated oil passes through microfiltration unit 62 having membranes with a 0.1 to 0.5 micron pore sizes.
  • the permeate (permeate I) is stocked in a storage tank 66.
  • variable speed gear pump 68 uses the permeate I has the feedstock to unit B.
  • the centrifugal pump 70 maintains a pressure superior to 125 psi up-stream of the microfiltration unit 72 having generally finer pore sizes than microfiltration unit 62.
  • the temperature is controlled by heat exchanger 74.
  • the recycled oil (Permeate II) is directed to holding tank 76.
  • the temperature and the circulation rate are again calculated in order to maintain a turbulent flow also corresponding to a Reynolds number superior to 2500 and preferably 3000.
  • the permeate II generally has a viscosity of 23.5 cSt at 40 °C. In units A and B, the viscosity of the circulation loop is controlled by the viscometers 78 and 80.
  • the advantage of the multi-stage system can be summarized in better viscosity control of the retentate and a product quality that is similar to commercial grade bitumen. Also, there is an increase of generally 5 to 10 % in the yield of the system based on weight recycled oil per volume of used oil when compared to a single stage system.
  • a distillation unit (atmospheric or vacuum) can be added up-stream or down-stream of the microfiltration unit, in either batch, continuous, or multi-stage systems, to separate the volatile fractions and the water vapor or to fractionate the permeate.
  • a distillation unit atmospheric or vacuum
  • the recycled oil (permeate) obtained from the microfiltration treatment of the present invention whether it be in batch, continous or multi ⁇ stage modes, has obvious qualities as specialty fuel oil.
  • the recycled retains a dark tint given to it mainly by halogenated hydrocarbons, as well as heterogenous, naphthalic, and aromatic compounds, and consequently is unsuitable to be re-used has a base oil for blended oils.
  • a decoloration post- treatment by adsorbents, such as alumina, clay or the like is then required.
  • FIG 6 illustrates an abso ⁇ tion unit 82 which can receive the permeate obtained following microfiltration.
  • the abso ⁇ tion unit 82 can, for example, be a packed column. Obviously other conventional designs are suitable.
  • the adsorbent used, such as alumina has a particle size generally inferior to 48 Mesh, to allow good contact with the recycled oil.
  • the abso ⁇ tion unit 82 generally operates at temperatures inferior to 200 °C and at pressures inferior to 150 psi.
  • the pressure is generated by pump 84.
  • Valve 86 is used to control the regenerated oil flow rate in function to the operating conditions. With such an arrangement, it is possible to obtain a regenerated oil with a yellow tint corresponding to a color indicae inferior to 3 according to ASTM D-1500 method. After this step, the regenerated oil can be recycled as part of a high quality lubricant.
  • FIG 7 shows an overall diagram of the used oil reclaiming system of the present invention, including its ancillary equipment. Firstly, used oil is transferred in a storage tank for quality control. The oil is then transferred to a second storage tank used to feed the system. In dotted lines there are shown optional distillation units used to separate the volatile fractions and water from the used oil stream. The permeate produced by the microfiltration system is routed to an adso ⁇ tion system to obtain a lube base stock of light tint. It is to be understood that various additives may be inco ⁇ orated at any point in the systems and methods of the present invention. The role of additives tends to enhance the used oil recycling process by lowering the viscosity of the used oil or to aid the microfiltration step.
  • a microfiltration loop was fed by a gear pump with used oil.
  • the oil was further heated to a temperature of at least 225 °C by an electrical heat exchanger with a capacity of 30 kW.
  • a centrifugal pump downstream of the heat exchanger and upstream of the microfiltration unit generated a pressure of approximately 150 psi at the entry of a stainless steel microfiltration unit having 0.2 micron pore size and a total filtration surface of
  • a used oil with an initial boiling point of 200 °C after distillation was processed using a continous mode of operation as shown in FIG 2 using a microfiltration unit equipped with ceramic membranes with a 0.2 micron pore size.
  • the operating pressure generated by a variable speed centrifugal pump, located upstream of the microfiltration unit, was initially set at 125 psi. Heating of the system was effected by an electrical heat exchanger with a capacity of 30 kW in order to obtain an start-up temperature of 200 °C in the circulation loop of used oil.
  • the pumping rate of the centrifugal pump and the temperature of the circulation loop were monitored and adjusted to maintain a state of turbulent flow of used oil (Reynolds number superior to 3000).
  • the Reynolds number is related to the viscosity of the fluid and the rate of pumping, a temperature increase will decrease the viscosity which will in turn increase the Reynolds number for a given pump speed.
  • the viscosity of the retentate increased as impurities collected in the circulation loop.
  • the temperature was adjusted to a maximum of 275 °C and the pump pressure to a maximum of 150 psi.
  • the Reynolds number finally dropped below 2500, the system was flushed of the retentate by an automatic signal coming from the viscometer 48 on the motorised valve 36 and further used oil was permitted to enter the circulation loop.
  • Table 2 Comparative analysis of used oil and of permeate obtained by microfiltration.
  • This example used a two-stage cascading unit as illustrated in FIG 5.
  • Used oil with a viscosity of 36 cSt at 40 °C was injected by a variable speed gear pump at a maximum rate of 10 GPM into the microfiltration unit A.
  • the centrifugal pump maintained a pressure of 150 psi upstream of the microfiltration unit equipped with stainless steel membranes.
  • An electrical heat exchanger with a capacity of 30 kW kept the temperature of the circulation flow superior to 200 °C.
  • the circulation loop flow rate and temperature were calculated according to the viscosity of the oil so that turbulent flow (Reynolds number superior to 2500 and preferably 3000) was maintained. Temperature was gradually increased to a maximum of 275 °C to reduce the viscosity in the circulation loop.
  • the heated oil was passed through the stainless steel microfiltration membranes having 0.5 micron pore size.
  • the permeate (permeate I) was produced at a rate of 17.1 GFD and was stocked in a tank for subsequent analysis.
  • the yield of the operation was 92 to 97 % volume of total recuperable lubricant fraction.
  • a second variable speed gear pump introduced the permeate I as feedstock of the second stage Unit B.
  • the centrifugal pump maintained a pressure of 150 psi upstream of the microfiltration unit, the latter equipped with stainless steel membranes having 0.2 micron pore size.
  • the temperature was controlled by an electrical heat exchanger with a capacity of 30 kW.
  • the temperature and pumping rate in the circulation loop were calculated in order to maintain a turbulent flow rate.
  • the permeate II produced at a rate of 18 GFD has a viscosity of 23.5 cSt at 40 °C.
  • the permeate II was passed through a upright catalytic adsorbent column containing particles of aluminum oxide, said column having a height of 30 cm and a diameter of 5 cm.
  • the particle size of aluminum oxide used was mesh 24.
  • the column was operated under a pressure of 40 psi and a temperature of 70 °C.
  • the resulting recycled oil obtained had a color indicae less than 3 as calculated from the ASTM-D1500 method. Table 3 presents the data obtained. Table 3: Results of microfiltration and abso ⁇ tion

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (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)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

Appareil et procédé de recyclage d'huile usée. L'appareil comprend une conduite d'alimentation dans laquelle une charge d'alimentation composée d'huile usée est introduite, une pompe de circulation permettant de pomper un courant d'huile usée à une pression d'au moins 105 psi, un échangeur de chaleur servant à chauffer le courant d'huile usée à une température comprise entre 200 °C et 500 °C, et au moins un organe de microfiltration contenant une pluralité de membranes de microfiltration dont la grosseur des pores est comprise entre 0,1 et 0,5 microns, permettant de microfiltrer le courant d'huile usée et d'en séparer un perméat d'huile recyclée tout en retenant un rétentat d'huile usée devant être recyclé dans le système. Au cours du fonctionnement de l'appareil, le courant d'huile usée en amont de l'organe de microfiltration est régulé, par la surveillance de la température ou de la pression dans le système, de façon à être maintenu à un débit correspondant à un nombre de Reynolds d'au moins 2300.
PCT/CA1994/000524 1993-09-22 1994-09-22 Microfiltration d'huile usee Ceased WO1995008609A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU77361/94A AU7736194A (en) 1993-09-22 1994-09-22 Microfiltration of used oil

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US12512793A 1993-09-22 1993-09-22
US08/125,127 1993-09-22

Publications (1)

Publication Number Publication Date
WO1995008609A1 true WO1995008609A1 (fr) 1995-03-30

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PCT/CA1994/000524 Ceased WO1995008609A1 (fr) 1993-09-22 1994-09-22 Microfiltration d'huile usee

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AU (1) AU7736194A (fr)
CA (1) CA2172391A1 (fr)
WO (1) WO1995008609A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7208079B2 (en) * 2002-07-30 2007-04-24 Nouredine Fakhri Process for the treatment of waste oils
WO2018121828A1 (fr) 2016-12-28 2018-07-05 Ocean Team Group A/S Centrale électrique dotée d'un système de nettoyage d'huile de lubrification et procédé de fonctionnement de la centrale électrique
WO2021216226A1 (fr) * 2020-04-20 2021-10-28 Exxonmobil Research And Engineering Company Séparation par membrane d'huile usagée et compositions produites

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3990963A (en) * 1974-03-06 1976-11-09 Institut Francais Du Petrole, Des Carburants Et Lubrifiants Et Entreprise De Recherches Et D'activities Petrollieres Elf Process for regenerating used lubricating oils
US4179019A (en) * 1978-01-09 1979-12-18 Danziger Harry Lee Apparatus for reclaiming used lubricating oils
EP0041013A1 (fr) * 1980-05-22 1981-12-02 COMMISSARIAT A L'ENERGIE ATOMIQUE Etablissement de Caractère Scientifique Technique et Industriel Procédé de traitement par ultrafiltration à température élevée d'une charge hydrocarbonée
EP0217534A2 (fr) * 1985-08-28 1987-04-08 National Research Council of Canada Procédé d'élimination de substances à partir de liquides hydrocarbonés d'origine fossile
JPH04145930A (ja) * 1990-10-04 1992-05-19 Toshiba Ceramics Co Ltd セラミックフィルタによる濾過方法
US5209838A (en) * 1991-10-07 1993-05-11 Aluminum Company Of America Purification of an oil-containing liquid using a surface treated permeable inorganic membrane

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3990963A (en) * 1974-03-06 1976-11-09 Institut Francais Du Petrole, Des Carburants Et Lubrifiants Et Entreprise De Recherches Et D'activities Petrollieres Elf Process for regenerating used lubricating oils
US4179019A (en) * 1978-01-09 1979-12-18 Danziger Harry Lee Apparatus for reclaiming used lubricating oils
EP0041013A1 (fr) * 1980-05-22 1981-12-02 COMMISSARIAT A L'ENERGIE ATOMIQUE Etablissement de Caractère Scientifique Technique et Industriel Procédé de traitement par ultrafiltration à température élevée d'une charge hydrocarbonée
EP0217534A2 (fr) * 1985-08-28 1987-04-08 National Research Council of Canada Procédé d'élimination de substances à partir de liquides hydrocarbonés d'origine fossile
JPH04145930A (ja) * 1990-10-04 1992-05-19 Toshiba Ceramics Co Ltd セラミックフィルタによる濾過方法
US5209838A (en) * 1991-10-07 1993-05-11 Aluminum Company Of America Purification of an oil-containing liquid using a surface treated permeable inorganic membrane

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Section Ch Week 9226, Derwent World Patents Index; Class J01, AN 92-214442 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7208079B2 (en) * 2002-07-30 2007-04-24 Nouredine Fakhri Process for the treatment of waste oils
WO2018121828A1 (fr) 2016-12-28 2018-07-05 Ocean Team Group A/S Centrale électrique dotée d'un système de nettoyage d'huile de lubrification et procédé de fonctionnement de la centrale électrique
AU2017389983B2 (en) * 2016-12-28 2024-02-01 Ikm Ocean Team A/S A power plant with a lubrication oil cleaning system and a method of operating the power plant
WO2021216226A1 (fr) * 2020-04-20 2021-10-28 Exxonmobil Research And Engineering Company Séparation par membrane d'huile usagée et compositions produites

Also Published As

Publication number Publication date
CA2172391A1 (fr) 1995-03-30
AU7736194A (en) 1995-04-10

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