WO1997026314A1 - Method for processing used lubricating oils in a dispersed aqueous phase for recycling - Google Patents
Method for processing used lubricating oils in a dispersed aqueous phase for recycling Download PDFInfo
- Publication number
- WO1997026314A1 WO1997026314A1 PCT/FR1997/000051 FR9700051W WO9726314A1 WO 1997026314 A1 WO1997026314 A1 WO 1997026314A1 FR 9700051 W FR9700051 W FR 9700051W WO 9726314 A1 WO9726314 A1 WO 9726314A1
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- oils
- oil
- water
- mixing tank
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- 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.)
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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
Definitions
- the present invention relates to a process for treating used (or used) lubricating oils to allow their recycling.
- Used lubricating oils come mainly from the draining process of automobile engines. These used oils are extremely toxic and a law requires their collection and disposal in approved centers throughout Europe.
- Used oil also known as engine drain oil, is made up of additives to which are added the soiling due to the operation of the engines at operating temperatures (+ 300 ° C).
- this oil contains volatile constituents (water, petrol, diesel), oil-soluble compounds formed by oxidation (resins, metallic soaps, viscosity index additives, organometallic compounds), insoluble compounds in oils (carbon particles, atmospheric dust, metals, metal oxides, lead oxides kept in suspension by oil detergents), additives containing a metal, dispersing additives, ashless additives, antioxidant additives and anti-corrosion, metals from pipes or fittings (iron, copper, lead), bearings (silver, cadmium), fuels (tetraethyl lead, among others).
- the oil deteriorates and becomes colored by oxidizing action in engines, by the formation of colored varnishes and the action of sulfur.
- the stains are fixed on the bleaching earth by creating a waste called "acid earth” which is then burned in an oven.
- the amount of bleaching earth represents approximately 30% of the oil used, used oil also called drain oil. It traps part of the oil and its subsequent burning is a source of nuisance.
- the separation of oil and earth is done in filter presses or in filters with continuous separation. The yield is of the order of 70% of the oil used (draining oil free of water). Between the bottom of the column and the head are plates to obtain various oil cups, viscosity ranging from 15 to 300 centistokes at 40 ° C.
- the oil obtained is then distilled under vacuum in tray columns; a pitch is collected at the bottom of the column containing heavy metals not separated by the action of sulfuric acid and treatment with earth. This pitch is to burn.
- the light products from petrol are collected, and especially unburned diesel in automobile engines.
- the amount of diesel produced from the used oils used is estimated at 10% on average.
- the present invention relates to a treatment making it possible to obtain, from used oils, oils comparable to virgin oils by extraction of the pollutants in dispersed phase of the water in oil emulsion type. It has been found that the emulsification and the shearing effect induce molecular deformations or changes in molecular structure which make it possible, without catalyst action, to obtain reactions hitherto impossible. Thus, it is possible to complex products which are incompatible with one another. The extraction of heavy metals and metalloids thus becomes possible.
- This method makes it possible to make reactive all homogeneous or heterogeneous products, to produce a molecular rupture, to make compatible all incompatible products, to favor the reactions, to make them reversible or irreversible, to favor inaccessible treatments, this without using pressure. Indeed, this process does not use sulfuric acid, no soda and reduces waste to less than 3% of the mass of oil treated.
- the used oil is filtered at 300 microns and then sent by means of a ball pump to an emulsifier. About 90% of used oil and 10% of water are introduced into the emulsifier at the same time in order to create a microemulsion.
- the remover is a device commonly used in the food industry to make mayonnaises and in the cosmetic industry to make creams; he works under very low pressure so as not to degrade the products he treats.
- the device consists of a motor driving toothed wheels which generate a strong shearing and dispersing effect producing a microemulsion.
- This micro-emulsion of water in oil is used to pass heavy metals and metalloids by diffusion from the organic phase to the aqueous phase. Indeed, it is almost impossible to complex the heavy metals in the organic phase while it is possible to complex these same heavy metals and these metalloids in the aqueous phase.
- This microemulsion is then pumped to a mixing tank into which a complexing agent for heavy metals and metalloids is injected by a metering pump, the whole microemulsion and complexing agent stirred for a certain time so that the contact is optimum and the metals heavy and the metalloids are complexed in the aqueous phase of the microemulsion.
- the complexing agent for heavy metals and metalloids is a product commonly used in the chemical industry.
- This entire emulsified phase is then pumped to a heat exchanger to make it reach 80 ° C. then pumped to a centrifuge. Centrifuging the emulsion gives three products or phases:
- phase 2 sediments and precipitates of heavy metals and metalloids
- the action of the heavy metal complexing agent on the emulsion followed by centrifugation gives a reduction greater than 90% of the heavy metals and the metalloids.
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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)
- Fats And Perfumes (AREA)
Abstract
Description
PROCEDE DE TRAITEMENT DES HUILES DE LUBRIFICATION USAGEES EN PHASE AQUEUSE DISPERSEE POUR LEUR RECYCLAGE PROCESS FOR THE TREATMENT OF LUBRICATING OILS USED IN AQUEOUS DISPERSE PHASE FOR RECYCLING
La présente invention concerne un procédé de traitement des huiles de lubrification usagées (ou usées) pour permettre leur recyclage.The present invention relates to a process for treating used (or used) lubricating oils to allow their recycling.
Les huiles de lubrification usagées proviennent principalement de l'opération de vidange des moteurs automobiles. Ces huiles usagées sont extrêmement toxiques et une loi impose leur collecte et leur élimination en centres agréés dans toute l'Europe.Used lubricating oils come mainly from the draining process of automobile engines. These used oils are extremely toxic and a law requires their collection and disposal in approved centers throughout Europe.
L'huile usagée, dite aussi huile de vidange des moteurs, se compose d'additifs auxquels viennent s'ajouter les souillures dues au fonctionnement des moteurs aux températures de fonctionnement (+ de 300°C). En fait, cette huile contient des constituants volatils (eau, essence, gazole), des composés solubles dans l'huile formés par oxydation, (résines, savons métalliques, additifs d'indice de viscosité, composés organo-métalliques), des composés insolubles dans les huiles (particules de carbone, poussières atmosphériques, métaux, oxydes métalliques, oxydes de plomb maintenus en suspension par les détergents de l'huile), des additifs renfermant un métal, des additifs dispersants, des additifs sans cendre, des additifs antioxydants et anti-corrosifs, des métaux provenant des canalisations ou des raccords (fer, cuivre, plomb), des coussinets (argent, cadmium), des carburants (plomb tétraethyle, entre autres).Used oil, also known as engine drain oil, is made up of additives to which are added the soiling due to the operation of the engines at operating temperatures (+ 300 ° C). In fact, this oil contains volatile constituents (water, petrol, diesel), oil-soluble compounds formed by oxidation (resins, metallic soaps, viscosity index additives, organometallic compounds), insoluble compounds in oils (carbon particles, atmospheric dust, metals, metal oxides, lead oxides kept in suspension by oil detergents), additives containing a metal, dispersing additives, ashless additives, antioxidant additives and anti-corrosion, metals from pipes or fittings (iron, copper, lead), bearings (silver, cadmium), fuels (tetraethyl lead, among others).
La liste des produits cités n'est pas limitative mais donnée à titre d'exemple. Les descriptions sont données à titre illustratif mais non limitatif.The list of products mentioned is not exhaustive but given as an example. The descriptions are given by way of illustration but not limitation.
L'huile s'altère et se colore par action oxydante dans les moteurs, par formation de vernis colorés et action du soufre.The oil deteriorates and becomes colored by oxidizing action in engines, by the formation of colored varnishes and the action of sulfur.
L'élimination des métaux lourds, des métalloïdes, des produits complexes, des goudrons, des résidus colloïdaux et autres contenus dans les huiles usagées des moteurs est réalisée actuellement par action combinée de la chaleur, de l'acide sulfurique, des terres décolorantes, de la filtration, de la centrifugation, de la distillation.The elimination of heavy metals, metalloids, complex products, tars, colloidal residues and other content in used engine oils is currently carried out by the combined action of heat, sulfuric acid, bleaching earth, filtration, centrifugation, distillation.
Les souillures se fixent sur les terres décolorantes en créant un déchet dénommé « terre acide » qui est ensuite brûlé dans un four. La quantité de terre décolorante représente environ 30 % de l'huile mise en oeuvre, huile usagée appelée aussi huile de vidange. Elle piège une partie de l'huile et son brûlage ultérieur est une source de nuisance. Généralement la séparation de l'huile et des terres se fait dans des filtres-presses ou dans des filtres à séparation continue. Le rendement est de l'ordre de 70 % de l'huile mise en jeu (huile de vidange exempte d'eau). Entre le pied de colonne et la tête s'étagent des plateaux permettant d'obtenir diverses coupes d'huile, de viscosité allant de 15 à 300 centistokes à 40°C.The stains are fixed on the bleaching earth by creating a waste called "acid earth" which is then burned in an oven. The amount of bleaching earth represents approximately 30% of the oil used, used oil also called drain oil. It traps part of the oil and its subsequent burning is a source of nuisance. Generally the separation of oil and earth is done in filter presses or in filters with continuous separation. The yield is of the order of 70% of the oil used (draining oil free of water). Between the bottom of the column and the head are plates to obtain various oil cups, viscosity ranging from 15 to 300 centistokes at 40 ° C.
Compte tenu des investissements mis en jeu, du faible rendement obtenu, de la nécessité de brûler brais et terres acides, ce procédé perd de plus en plus d'intérêt malgré les améliorations apportées et aussi face au prix bas des huiles.Given the investments involved, the low yield obtained, the need to burn pitches and acidic soils, this process is losing more and more interest despite the improvements made and also faced with the low price of oils.
L'huile obtenue est ensuite distillée sous vide dans des colonnes à plateaux ; on recueille en fond de colonne un brai contenant des métaux lourds non séparés par action de l'acide sulfurique et du traitement à la terre. Ce brai est à brûler. En tête de la colonne on recueille les légers provenant des essences, et surtout des gazoles non brûlés dans les moteurs automobiles. On estime à 10 % en moyenne la quantité de gazole produite à partir des huiles usagées mises en oeuvre.The oil obtained is then distilled under vacuum in tray columns; a pitch is collected at the bottom of the column containing heavy metals not separated by the action of sulfuric acid and treatment with earth. This pitch is to burn. At the head of the column, the light products from petrol are collected, and especially unburned diesel in automobile engines. The amount of diesel produced from the used oils used is estimated at 10% on average.
L'exposé de l'invention et des revendications résoud à la fois le problème économique et le problème de nuisance.The description of the invention and the claims solves both the economic problem and the nuisance problem.
La présente invention concerne un traitement permettant d'obtenir, à partir d'huiles usagées, des huiles comparables à des huiles vierges par extraction des polluants en phase dispersée de type emulsion eau dans huile. On a constaté que la mise en emulsion et l'effet de cisaillement induisent des déformations moléculaires ou des changements de structure moléculaire qui permettent, sans action de catalyseur, d'obtenir des réactions jusque là impossibles. Ainsi, il est possible de complexer des produits incompatibles entre eux. L'extraction des métaux lourds et des métalloïdes devient ainsi possible. Cette méthode permet de rendre réactifs tous produits homogènes ou hétérogènes, de produire une rupture moléculaire, de rendre compatibles tous produits incompatibles, de favoriser les réactions, de les rendre réversibles ou irréversibles, de favoriser des traitements inaccessibles, ceci sans utiliser la pression. En effet, ce procédé n'utilise pas d'acide sulfurique, pas de soude et réduit les déchets à moins de 3 % de la masse d'huile traitée.The present invention relates to a treatment making it possible to obtain, from used oils, oils comparable to virgin oils by extraction of the pollutants in dispersed phase of the water in oil emulsion type. It has been found that the emulsification and the shearing effect induce molecular deformations or changes in molecular structure which make it possible, without catalyst action, to obtain reactions hitherto impossible. Thus, it is possible to complex products which are incompatible with one another. The extraction of heavy metals and metalloids thus becomes possible. This method makes it possible to make reactive all homogeneous or heterogeneous products, to produce a molecular rupture, to make compatible all incompatible products, to favor the reactions, to make them reversible or irreversible, to favor inaccessible treatments, this without using pressure. Indeed, this process does not use sulfuric acid, no soda and reduces waste to less than 3% of the mass of oil treated.
L'huile usagée est filtrée à 300 microns puis envoyée par le biais d'une pompe à boisseau vers un émulsionneur. Il est introduit en même temps dans l'émulsionneur environ 90 % d'huile usagée et 10 % d'eau afin de créer une micro-émulsion. L'émuisionneur est un appareil utilisé couramment dans l'industrie agro¬ alimentaire pour confectionner des mayonnaises et dans l'industrie cosmétique pour confectionner des crèmes ; il travaille sous très faible pression afin de ne pas dégrader les produits qu'il traite. L'appareil est constitué d'un moteur entraînant des roues dentées qui génèrent un fort effet de cisaillement et de dispersion produisant une micro-émulsion.The used oil is filtered at 300 microns and then sent by means of a ball pump to an emulsifier. About 90% of used oil and 10% of water are introduced into the emulsifier at the same time in order to create a microemulsion. The remover is a device commonly used in the food industry to make mayonnaises and in the cosmetic industry to make creams; he works under very low pressure so as not to degrade the products he treats. The device consists of a motor driving toothed wheels which generate a strong shearing and dispersing effect producing a microemulsion.
Cette micro-émulsion d'eau dans l'huile sert à faire passer les métaux lourds et les métalloïdes par diffusion de la phase organique à la phase aqueuse. En effet, il est quasiment impossible de complexer les métaux lourds en phase organique alors qu'il est possible de complexer ces mêmes métaux lourds et ces métalloïdes en phase aqueuse.This micro-emulsion of water in oil is used to pass heavy metals and metalloids by diffusion from the organic phase to the aqueous phase. Indeed, it is almost impossible to complex the heavy metals in the organic phase while it is possible to complex these same heavy metals and these metalloids in the aqueous phase.
Cette micro-émulsion est ensuite pompée vers un bac de mélange dans lequel un complexant des métaux lourds et métalloïdes est injecté par une pompe doseuse, l'ensemble micro-émulsion et complexant agité un certain temps afin que le contact soit optimum et que les métaux lourds et les métalloïdes soient complexés dans la phase aqueuse de la micro-émulsion.This microemulsion is then pumped to a mixing tank into which a complexing agent for heavy metals and metalloids is injected by a metering pump, the whole microemulsion and complexing agent stirred for a certain time so that the contact is optimum and the metals heavy and the metalloids are complexed in the aqueous phase of the microemulsion.
Le complexant des métaux lourds et des métalloïdes est un produit couramment utilisé dans l'industrie chimique.The complexing agent for heavy metals and metalloids is a product commonly used in the chemical industry.
L'ensemble de cette phase émulsifiée est ensuite pompé vers un echangeur thermique afin de lui faire atteindre 80°C. puis pompé vers une centrifugeuse. La centrifugation de l'émulsion donne trois produits ou phases :This entire emulsified phase is then pumped to a heat exchanger to make it reach 80 ° C. then pumped to a centrifuge. Centrifuging the emulsion gives three products or phases:
- phase 1 - eau + métaux lourds + métalloïdes,- phase 1 - water + heavy metals + metalloids,
- phase 2 - sédiments et précipités des métaux lourds et métalloïdes,- phase 2 - sediments and precipitates of heavy metals and metalloids,
- phase 3 - huile démétallisée (produit noble) prête pour une distillation sous vide.- phase 3 - demetallized oil (noble product) ready for vacuum distillation.
L'action du complexant des métaux lourds sur l'émulsion suivie d'une centrifugation donne une réduction supérieure à 90 % des métaux lourds et des métalloïdes.The action of the heavy metal complexing agent on the emulsion followed by centrifugation gives a reduction greater than 90% of the heavy metals and the metalloids.
L'extraction de la plus grande partie des métaux lourds et métalloïdes ainsi que la séparation de l'eau et des matières solides par centrifugation permettent d'obtenir une huile démétallisée et pré-traitée. Cette qualité d'huile est absolument nécessaire dans le cadre des opérations de traitements utérieurs permettant d'obtenir une huile de base aux caractéristiques comparables à celles d'une huile de lubrification vierge. Les colonnes de distillation-fractionnement récentes sont de type à garnitures. L'huile qu'elles distillent doit être le plus épuré possible afin d'éviter le colmatage des garnitures ainsi que les chutes de rendement de distillation.The extraction of most of the heavy metals and metalloids as well as the separation of water and solid materials by centrifugation make it possible to obtain a demetallized and pre-treated oil. This quality of oil is absolutely necessary within the framework of subsequent treatment operations making it possible to obtain a base oil with characteristics comparable to those of a virgin lubricating oil. Recent distillation-fractionation columns are of the packing type. The oil they distill must be as pure as possible in order to avoid clogging of the linings as well as drops in distillation yield.
En cas d'hydrogénation de cette huile lors d'une phase ultérieure, son pré-traitement permet de préserver le catalyseur de la pollution par les métaux lourds et les métalloïdes de type soufrés. A titre d'exemples illustratifs, mais non limitatifs, on peut citer, par application de ce procédé :In the event of hydrogenation of this oil during a subsequent phase, its pre-treatment makes it possible to preserve the catalyst from pollution by heavy metals and metalloids of the sulfur type. By way of illustrative but nonlimiting examples, there may be mentioned, by application of this process:
- l'élimination des métaux lourds,- elimination of heavy metals,
- l'élimination des métalloïdes,- elimination of metalloids,
- l'élimination des produits complexes provenant des additifs des huiles,- the elimination of complex products from oil additives,
- l'élimination des résidus collo'idaux ou autres,- the disposal of residues colloid idaux or other,
- la précipitation des produits d'oxydation. - precipitation of oxidation products.
Claims
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR9600469A FR2743570B1 (en) | 1996-01-17 | 1996-01-17 | PROCESS FOR THE TREATMENT OF LUBRICATING OILS USED IN AQUEOUS DISPERSE PHASE FOR RECYCLING |
| FR96/00469 | 1996-01-17 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO1997026314A1 true WO1997026314A1 (en) | 1997-07-24 |
Family
ID=9488170
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/FR1997/000051 Ceased WO1997026314A1 (en) | 1996-01-17 | 1997-01-13 | Method for processing used lubricating oils in a dispersed aqueous phase for recycling |
Country Status (2)
| Country | Link |
|---|---|
| FR (1) | FR2743570B1 (en) |
| WO (1) | WO1997026314A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2795421A1 (en) * | 1999-06-23 | 2000-12-29 | Richard Deutsch | Decontamination of waste semi-synthetic or synthetic mineral oils comprises treatment with glycol, chelating agents, and barium hydroxide before ultimate fractional distillation and possible decoloration treatment |
| RU2556641C1 (en) * | 2014-08-06 | 2015-07-10 | Государственное научное учреждение Всероссийский научно-исследовательский институт использования техники и нефтепродуктов Российской академии сельскохозяйственных наук (ГНУ ВНИИТиН Россельхозакадемии) | Method of purifying waste synthetic motor oil |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6117309A (en) * | 1997-09-08 | 2000-09-12 | Probex Corporation | Method of rerefining waste oil by distillation and extraction |
| CN113004969A (en) * | 2021-02-27 | 2021-06-22 | 新疆佳宇恒能源科技有限公司 | Hydrogenation method for regeneration of waste lubricating oil |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB233334A (en) * | 1924-04-29 | 1926-10-21 | Sharples Specialty Co | Improvements in or relating to processes of purifying oil |
| US1770736A (en) * | 1924-11-28 | 1930-07-15 | Nevin E Funk | Oil water washer |
| GB374915A (en) * | 1931-03-09 | 1932-06-09 | Stone J & Co Ltd | Improvements in and connected with the separation of collcidal and other suspensionsfrom liquids |
| GB679914A (en) * | 1948-03-17 | 1952-09-24 | Frederick Charles Bersworth | Improvements in method of reclaiming the hydrocarbon content of used hydrocarbon lubricants |
| US5125966A (en) * | 1990-12-20 | 1992-06-30 | Nalco Chemical Company | Process for de-oiling mill sludge |
| WO1996000273A1 (en) * | 1994-06-23 | 1996-01-04 | Corex Technologies (1993) Ltd. | Process for the reclamation of used lubricating oils |
-
1996
- 1996-01-17 FR FR9600469A patent/FR2743570B1/en not_active Expired - Fee Related
-
1997
- 1997-01-13 WO PCT/FR1997/000051 patent/WO1997026314A1/en not_active Ceased
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB233334A (en) * | 1924-04-29 | 1926-10-21 | Sharples Specialty Co | Improvements in or relating to processes of purifying oil |
| US1770736A (en) * | 1924-11-28 | 1930-07-15 | Nevin E Funk | Oil water washer |
| GB374915A (en) * | 1931-03-09 | 1932-06-09 | Stone J & Co Ltd | Improvements in and connected with the separation of collcidal and other suspensionsfrom liquids |
| GB679914A (en) * | 1948-03-17 | 1952-09-24 | Frederick Charles Bersworth | Improvements in method of reclaiming the hydrocarbon content of used hydrocarbon lubricants |
| US5125966A (en) * | 1990-12-20 | 1992-06-30 | Nalco Chemical Company | Process for de-oiling mill sludge |
| WO1996000273A1 (en) * | 1994-06-23 | 1996-01-04 | Corex Technologies (1993) Ltd. | Process for the reclamation of used lubricating oils |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2795421A1 (en) * | 1999-06-23 | 2000-12-29 | Richard Deutsch | Decontamination of waste semi-synthetic or synthetic mineral oils comprises treatment with glycol, chelating agents, and barium hydroxide before ultimate fractional distillation and possible decoloration treatment |
| WO2001000756A1 (en) * | 1999-06-23 | 2001-01-04 | Richard Deutsch | Method for decontaminating waste semi-synthetic or synthetic mineral oils |
| RU2556641C1 (en) * | 2014-08-06 | 2015-07-10 | Государственное научное учреждение Всероссийский научно-исследовательский институт использования техники и нефтепродуктов Российской академии сельскохозяйственных наук (ГНУ ВНИИТиН Россельхозакадемии) | Method of purifying waste synthetic motor oil |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2743570B1 (en) | 1998-03-06 |
| FR2743570A1 (en) | 1997-07-18 |
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