EP0572630B1 - Procede de regeneration d'huiles lubrifiantes usees - Google Patents
Procede de regeneration d'huiles lubrifiantes usees Download PDFInfo
- Publication number
- EP0572630B1 EP0572630B1 EP93901602A EP93901602A EP0572630B1 EP 0572630 B1 EP0572630 B1 EP 0572630B1 EP 93901602 A EP93901602 A EP 93901602A EP 93901602 A EP93901602 A EP 93901602A EP 0572630 B1 EP0572630 B1 EP 0572630B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- oil
- bleaching earth
- oils
- waste oil
- waste
- 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
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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
- C10M175/0008—Working-up used lubricants to recover useful products ; Cleaning with the use of adsorbentia
-
- 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
- C10M175/0033—Working-up used lubricants to recover useful products ; Cleaning by thermal processes using distillation processes; devices therefor
Definitions
- the present invention relates to a method for cleaning used Lubricating oils through vacuum distillation and two post-treatments of the lubricating oil distillate with finely divided, not activated Bleaching earth at 260 to 350 ° C.
- Lubricating oils are also produced which contain synthetic parts or only for special purposes consist of synthetic base oils.
- Waste oil must be disposed of properly in the Federal Republic of Germany, whereby according to the new waste law from 1.11.1986 the waste oil owner for the proper disposal is your own responsibility.
- the waste oil owner for the proper disposal is your own responsibility.
- For the end user engine oil and other lubricating oils have a right of free Return of used oils to the lubricating oil supplier.
- the material recycling The disposal of used oil is in the foreground. This means that by means of suitable processes from the used oil again lubricant base oil (Second refinery), the quality of which is obtained from crude oil lubricant base oil produced.
- waste oil is processed in the way that the waste oil is collected by collecting companies, for example Engine, hydraulic and gear oil are collected separately must be from types of oil such. B. metalworking oil.
- the collecting company delivers the waste oil to waste oil regeneration plants, so-called Second refining plants.
- Second refining plants only Used oils are processed that do not contain more than 0.2 wt .-% chlorine Contain more than 4 ppm polychlorinated biphenyls.
- the second refining process is the re-refining with more concentrated Sulfuric acid and bleaching earth.
- the waste oil is first freed from low boilers and water by distillation and then distilled over in vacuo.
- the distillate comes with concentrated sulfuric acid treated.
- the product treated in this way becomes the so-called spindle oil is distilled off over activated bleaching earth.
- Subsequently can be a purely adsorptive aftertreatment with activated Bleaching earth at approx. 120 ° C (see eg "Waste oil recycling, Klaus Müller, Erich Schmidt Verlag, Berlin, Bielefeld, page 104).
- the sulfuric acid / bleaching earth process has one considerable disadvantage that there is a so-called acid resin, a product that occurs when treating the waste oil with concentrated sulfuric acid settles as a difficult phase, cannot be deposited and is difficult to dispose of is.
- spent, loaded with sulfuric acid Bleaching earth in considerable quantities, which is also difficult to dispose of.
- the waste oil is first mixed with a finely divided metallic Sodium reacted and then also distilled over in vacuo.
- This process also requires chemical treatment but instead of concentrated sulfuric acid highly reactive fine distributed, metallic sodium is used.
- the waste oil is first mixed with a diammonium phosphate solution transferred.
- water and volatile hydrocarbons removed by distillation. Now with activated bleaching earth treated. This is followed by a hydrating one Refining.
- Bleaching earth has long been used to clean used oils.
- the bleaching earths are water-containing aluminum-magnesium silicates from the bentonite group, which are activated by boiling in hydrochloric acid; this dissolves soluble, basic fractions, such as CaO, MgO and also Fe 2 O 3, from the raw material and exposes the actual capillary structure of the adsorption material. They are also referred to as Walker, Fuller Florida earth or bentonite (Klaus Müller, waste oil recycling, Erich Schmidt Verlag GmbH, Berlin, 1982, page 96).
- GB-A-327,294 describes a process for refining used lubricating oils, according to which is treated with sulfuric acid after removal of water. Subsequently the oil is separated off, distilled in vacuo and with an adsorbent, preferably treated with Fuller soil.
- DE-OS 37 38 391 describes a process for evaporating waste oil under vacuum a special, complicated evaporation apparatus. The procedure exists from two stages. The second stage is the evaporation of gas oil and spindle oil described over bleaching earth under vacuum. From the. Distillation bottoms are obtained after Filter off the actual lubricating oil from the bleaching earth. A similar process is known from the application FR-A-2 322 918, being used as an adsorbent acid-activated and / or neutral bleaching earth is used.
- DD-PS 77553 describes a thermal pretreatment of waste oil before the hydrogenation Refining described. The filtration aid can be used before or after the heat treatment Bleaching earth can be added.
- the process consists of the cleaning of used oils by vacuum distillation, after-treatment with finely divided solids and subsequent separation of the solids, characterized in that the distilled oil in 2 stages with a total of 4 to 20 wt .-%, preferably 6 to 16 wt .-% with natural, untreated Bentonite-type bleaching earth in the temperature range from 280 to 330 ° C during a residence time of 5 to 120 min. is mixed thoroughly and then the Solid is separated.
- the low-boiling parts in the waste oil namely the low-boiling hydrocarbons and the water still present in the waste oil is distilled off.
- This can be done under Normal pressure take place, for example at a bottom temperature of about 160 ° C.
- One can however, also work under a slight vacuum, for example at 40 to 100 mbar.
- you can also use the medium oil and the spindle oil, i.e. the light lubricating oil fraction Remove by distillation in vacuo, at about 5 to 10 mbar and a bottom temperature of 210 ° C.
- the vacuum distillation apparatus be performed.
- Several distillation columns are known in where lubricating oil can be gently distilled, e.g. short-path evaporators and thin film evaporators.
- the vacuum is generally from 0.01 mbar to 20 mbar, preferably at 0.05 to 10 mbar.
- the spindle oil In the event that the spindle oil is not separated as already described, it can also be distilled off in another way. This can be done, for example, in such a way that one Vacuum distillation column, the spindle oil is distilled off overhead and the actual one Lube oil in the side trigger. However, the separation can also be carried out in such a way that in one column of spindle oil is separated by distillation and in another the actual one Lubricating oil.
- spindle oil is not used as an engine lubricating oil, but is used mainly used in hydraulic oils.
- the broad boiling range for lubricating oil lies between 350 ° C and 640 ° C, but there are also fractions with others Boiling ranges or viscosities distilled off, e.g. between 360 and 540 ° C or 390 and 515 ° C. Lubricator win distillation cuts in such a way that for certain Applications required boiling analysis or viscosity is observed.
- the lubricating oil obtained by vacuum distillation is now used according to the invention in a mixing apparatus discontinuously or continuously with fine distributed, not activated bleaching earth in two stages and at 280 to 330 ° C, during a dwell time of 5 to 120 min., preferably intimately mixed from 10 to 70 min. Subsequently the solid is separated off in each case.
- Different temperatures can also be used in the two treatment stages and residence times in the areas mentioned.
- Montmorillonite is known a major mineral of bentonite.
- Minerals also include mixtures with beidellite (smectite), nontronite, saponite or hectorite. Further can be present iron oxides such. B. hematite.
- the treatment is carried out with non-activated bleaching earth two-stage.
- the inventive method can of course also in more than two stages are carried out, however, the skilled person will do this from an economic point of view Avoid reasons if possible.
- One of the stages can also include adding non-activated bleaching earth a distillation column, provided that the additives and impurities containing sump has been removed. Furthermore falls in the invention Frame also the partial addition of activated bleaching earth, although those skilled in the art will refrain from doing so for economic reasons.
- the grain size of the bleaching earth used is not decisive Roll, but finely ground materials are preferred, for example from 30 to 60 mesh.
- the solids are in one wide grain size range, such as between 0.001 mm up to 1 mm or more, with a very fine distribution the residence time in general can be reduced and the amounts of added solid.
- the specialist has a wide range of options for selecting the grain size.
- the desired grain sizes according to the invention can also be smaller than the grain sizes mentioned Develop properties.
- any mixing vessels of the prior art can be used as mixing vessels will.
- the mixing devices can work continuously or discontinuously. So can be used up to mixing cascades, simple mixing tanks, Intensive stirring reactors, built-in mixing sections and numerous other.
- the specialist is free to do so depending on the a suitable plant size and other criteria Select mixing device. It is essential, however, that an intimate Contact between the waste oil to be cleaned and the solids used is achieved.
- Table 1 shows results according to the invention when cleaning three different ones Used oils I, II and III compiled. Are for comparison Analyzes and data of a typical waste oil compared.
- the table shows that excellent by the inventive method Values can be obtained regarding color, viscosity index, flash point, Ash, neutralization numbers, chlorine and phosphorus.
- the used Waste oils I, II and III have been taken over by various waste oil collectors.
- the Waste oil quality corresponds to that prescribed by law regarding chlorine and PCB content is mandatory.
- the reference old oil is a typical one Waste oil in the same category as waste oils I, II and III.
- lubricating oil data from used oil distillates are different Viscosities at 40 ° C and 100 ° C summarized.
- Under EP are data from used waste oil specified. It is a French waste oil. Distillates 1 and 2 were each once and twice with 6 wt .-% each non-activated bleaching earth at 320 ° C and a dwell time of 30 min each treated.
- Table 5 summarizes results from the treatment of a distillation cut from 390 to 515 ° C from a Spanish waste oil from the Barcelona area.
- a Spanish, non-activated, bentonite-based bleaching earth which contained saponite and 2 to 3% by weight of hematite was used as the bleaching earth.
- Sample a) is the untreated cut.
- Sample b) is the cut once treated with 6% by weight of bleaching earth at 320 ° C. and 30 minutes. The neutralization number is not satisfactory. However, very good values are obtained when treated twice (sample c). Analogously, 8% by weight of bleaching earth was used in samples d) and e).
- Sample f) was treated once with 8% by weight of bleaching earth, which was obtained from the 2nd treatment stage after filtering off. Neither color number nor neutralization number are satisfactory.
- Sample g) was treated in the first stage like sample f) and in stage 2 with 8% by weight of fresh bleaching earth. The values obtained are very good. This means that when using fresh bleaching earth in stage 2 and bleaching earth filtered off in stage 2, very good values are obtained. Good results were also obtained with this procedure with 4 and 6% by weight of bleaching earth. In general, the overall consumption of bleaching earth can be reduced accordingly.
- the figure shows an example of a process flow diagram with two solids cleaning stages shown.
- Waste oil flows over filter 1 to remove coarse impurities.
- the filtered waste oil flows into stripping column 3, from which a mixture of low-boiling hydrocarbons and water is distilled off at the top.
- separation tank 5 the water flows out of the system via 6, while the low-boiling hydrocarbons are collected in tank 7.
- the bottom from 3 flows into vacuum column 4, in which lubricating oil is distilled off overhead. 4 can also be operated in such a way that spindle oil is removed overhead and the actual lubricating oil is drawn off in the side draw.
- used lubricating oils can, as explained in detail mineral base, which can also contain synthetic oils and synthetic Lubricating oils based on hydrocarbons again to a flawless Second raffinate to be worked up.
- the present invention overcomes the prejudice of the person skilled in the art that when using bleaching earth for cleaning used oil distillates, portions such as CaO, MgO or Fe 2 O 3 have to be removed from the raw material in order to expose the capillary structure of the bleaching earth. Rather, the results according to the invention show that these proportions are even advantageous under the conditions according to the invention.
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)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Lubricants (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Claims (2)
- Procédé pour la purification des huiles usés par distillation sous vide, traitement supplémentaire avec des solides distribués fins et suivant la séparation des solides, caractérisé en ce que l'huile distillé est mélangé intense avec de tots ensemble 4 à 20 pour-cent de poids et de préférence de 6 à 16 pour-cent de poids de terre décolorante naturele et non-pretraitée du type bentonite, la température étant comprise entre 180 à 330°C à une durée de 5 à 120 minutes et ent ce que saivant les solides sont séparés.
- Procédé selon la revendication 1, caractérisé en ce quelle traitement avec la terre décolorante a une durée de 10 à 70 minutes.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4142829 | 1991-12-23 | ||
DE4142829A DE4142829C2 (de) | 1991-12-23 | 1991-12-23 | Verfahren zur Reinigung von gebrauchten Schmierölen |
PCT/DE1992/001074 WO1993013189A1 (fr) | 1991-12-23 | 1992-12-21 | Procede de regeneration d'huiles lubrifiantes usees |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0572630A1 EP0572630A1 (fr) | 1993-12-08 |
EP0572630B1 true EP0572630B1 (fr) | 1998-09-02 |
Family
ID=6448047
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP93901602A Expired - Lifetime EP0572630B1 (fr) | 1991-12-23 | 1992-12-21 | Procede de regeneration d'huiles lubrifiantes usees |
Country Status (8)
Country | Link |
---|---|
EP (1) | EP0572630B1 (fr) |
JP (1) | JPH06510562A (fr) |
AT (1) | ATE170548T1 (fr) |
BR (1) | BR9205666A (fr) |
CA (1) | CA2104578A1 (fr) |
DE (2) | DE4142829C2 (fr) |
NO (1) | NO932937D0 (fr) |
WO (1) | WO1993013189A1 (fr) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2757873B1 (fr) * | 1996-12-31 | 1999-03-19 | Total Raffinage Distribution | Procede de regeneration d'une fraction d'huile lubrifiante usee |
EP0926226A1 (fr) * | 1997-12-22 | 1999-06-30 | C.S. Filtration S.p.r.l. | Filtration d'huiles synthétiques par produit silico-calcaire |
US20030024856A1 (en) * | 2001-03-26 | 2003-02-06 | Phil Surana | Method for removal of oder from poly alpha-olefins |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB327294A (en) * | 1929-04-10 | 1930-04-03 | William Detwiller Harris | Method of refining used lubricating oil |
US2286369A (en) * | 1931-01-02 | 1942-06-16 | Bocji Corp | Method of purifying oil |
US2012695A (en) * | 1933-03-24 | 1935-08-27 | Quigley Co | Apparatus for reclaiming crank-case oil |
US2401339A (en) * | 1941-11-26 | 1946-06-04 | Buckeye Lab Corp | Treatment of oils and waxes |
US2446489A (en) * | 1945-03-21 | 1948-08-03 | Shell Dev | Process for regenerating spent internal-combustion engine lubricating oils |
US2496888A (en) * | 1947-01-22 | 1950-02-07 | De Witt H Palmer | Oil reconditioning or clarifying apparatus |
DE1545267A1 (de) * | 1966-05-26 | 1969-12-11 | Durbanolwerk Hans Durban Kg | Vorrichtung zur Raffination von Motoren- und Motorenaltoelen |
US4101414A (en) * | 1975-09-02 | 1978-07-18 | Unitech Chemical Inc. | Rerefining of used motor oils |
DE3738391A1 (de) * | 1987-11-12 | 1989-05-24 | Wilhelm Joachim A Dr Ing | Verfahren zum destillativen entfernen von verunreinigungen aus altoel |
-
1991
- 1991-12-23 DE DE4142829A patent/DE4142829C2/de not_active Expired - Fee Related
-
1992
- 1992-12-21 AT AT93901602T patent/ATE170548T1/de not_active IP Right Cessation
- 1992-12-21 EP EP93901602A patent/EP0572630B1/fr not_active Expired - Lifetime
- 1992-12-21 DE DE59209484T patent/DE59209484D1/de not_active Expired - Fee Related
- 1992-12-21 CA CA002104578A patent/CA2104578A1/fr not_active Abandoned
- 1992-12-21 BR BR9205666A patent/BR9205666A/pt not_active Application Discontinuation
- 1992-12-21 JP JP5511349A patent/JPH06510562A/ja active Pending
- 1992-12-21 WO PCT/DE1992/001074 patent/WO1993013189A1/fr active IP Right Grant
-
1993
- 1993-08-18 NO NO932937A patent/NO932937D0/no unknown
Also Published As
Publication number | Publication date |
---|---|
NO932937L (no) | 1993-08-18 |
DE59209484D1 (de) | 1998-10-08 |
DE4142829C2 (de) | 1994-08-25 |
NO932937D0 (no) | 1993-08-18 |
WO1993013189A1 (fr) | 1993-07-08 |
JPH06510562A (ja) | 1994-11-24 |
ATE170548T1 (de) | 1998-09-15 |
BR9205666A (pt) | 1994-05-17 |
EP0572630A1 (fr) | 1993-12-08 |
DE4142829A1 (de) | 1993-06-24 |
CA2104578A1 (fr) | 1993-06-24 |
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