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EP0377606B1 - Verfahren zur reinigung und regenerierung von altölen - Google Patents

Verfahren zur reinigung und regenerierung von altölen Download PDF

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Publication number
EP0377606B1
EP0377606B1 EP88907226A EP88907226A EP0377606B1 EP 0377606 B1 EP0377606 B1 EP 0377606B1 EP 88907226 A EP88907226 A EP 88907226A EP 88907226 A EP88907226 A EP 88907226A EP 0377606 B1 EP0377606 B1 EP 0377606B1
Authority
EP
European Patent Office
Prior art keywords
oil phase
temperature
oil
pretreated
solution
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
EP88907226A
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German (de)
English (en)
French (fr)
Other versions
EP0377606A1 (de
Inventor
Adekunle Onabajo
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.)
RWE Entsorgung AG
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RWE Entsorgung AG
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Filing date
Publication date
Application filed by RWE Entsorgung AG filed Critical RWE Entsorgung AG
Priority to AT88907226T priority Critical patent/ATE82769T1/de
Publication of EP0377606A1 publication Critical patent/EP0377606A1/de
Application granted granted Critical
Publication of EP0377606B1 publication Critical patent/EP0377606B1/de
Anticipated expiration legal-status Critical
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
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
    • C10G2400/10—Lubricating oil

Definitions

  • the invention relates to a process for cleaning and regenerating used oils, in particular used lubricating oils, by filtration, heat treatment and stripping off the low boilers consisting of solvent and water.
  • Waste oils are used mineral oils, especially used engine and lubricating oils.
  • the utility value of mineral lubricating oils is greatly affected by oxidation products, pollution and other additives that accumulate during use. Such products no longer fully fulfill their task and must be replaced. They are referred to as waste oils and are collected and processed for reasons of environmental protection, raw material conservation and also from an economic point of view.
  • Waste oils mainly consist of a base oil based on mineral oil or synthetic oil, but contain considerable amounts of foreign substances, e.g. As water, solvents, fuels, asphalt-like substances, acids, resins, ashes and additives such as antioxidants, anti-corrosion agents, wetting agents, dispersants, anti-foaming agents and viscosity index improvers.
  • the additives can contain halogen, sulfur and nitrogen compounds and numerous other, partly toxic components.
  • Waste oils are first cleaned mechanically by separating undissolved impurities and foreign substances by sedimentation, filtration or centrifugation. The separation can be accelerated considerably by heating the used oil to 50 to 100 ° C.
  • Waste oil is subjected to a refining hydrogenation over nickel-molybdenum catalysts after pretreatment with an aqueous diammonium phosphate solution.
  • polychlorinated biphenyls are also said to be at least partially degraded in this process, chlorinated solvents and cleaning liquids, metalworking oils and other processing oils and their composition are intended for the regeneration of this process is not clearly identified, and insulating and transformer oils have not been preserved in the feed. Suitable starting products for this process are therefore essentially used engine oils.
  • the waste oil is freed of water and dirt by sedimentation and residual water and low boilers by atmospheric distillation.
  • the gas oil fraction is then separated off in a separate stage.
  • the lubricating oil components are fractionated, condensed and dirt, additives and some of the oxidation products are removed as sump.
  • the distillates are hydrofinished and stripped. Since acid refining is also absent in this process, additives or foreign components must either be separable by distillation or convertible by hydrogenation. Ingredients must not affect the activity of the hydrogenation catalyst, so that, for. B. Cutting oils with contents of halogenated hydrocarbons cannot be processed by this method either, see Ullmanns Encyklopadie der Technische Chemie, 4th edition volume 20, page 500.
  • the oxidation products and additives are also not removed with sulfuric acid, but by treatment with finely dispersed sodium, whereby they either polymerize or are converted into sodium salts which have a boiling point so high that the oil is distilled can.
  • the distillation takes place in two steps, the second of which is designed as a short-path thin-film evaporation for separating the reaction products.
  • the invention has for its object to develop a universally applicable method that allows pollutants and other undesirable components from used lubricating oils and other waste oils with higher product yields and higher product quality with less process effort and in particular less landfill than what is possible according to the prior art remove.
  • the process is said to be particularly suitable for special treatments, the hydrogenation or, for example, the treatment with sodium and to bring about simplifications in terms of process technology and the associated cost reductions, for example by avoiding catalyst poisoning when the hydrogenation stage is switched on.
  • process stage (2) dewatering takes place in particular.
  • the feed materials bind the water as residue sludge, which is then separated in a known manner by separation. 50 to 80% of the free water present in the waste oil is separated in this way.
  • the residual water and the low boilers are then removed by distillation in process step (3).
  • the waste oil treatment according to process steps (1) to (3) takes place in a temperature range from 50 to 140 ° C, with temperatures as low as possible being preferred in this range.
  • PCB accumulation in the low boilers and water is excluded, since the boiling point range of polychlorinated bi- and terphenylene is above the stripping temperature. PCB separation therefore does not take place in process stage (3), which ensures that the low boilers and water obtained by this process are not contaminated with PCB. This is of great importance for an environmentally friendly process for waste oil processing.
  • Process stage 3 can also be carried out before process stage 2 by first separating the low boilers from the mixture obtained, then letting them settle in a decanter and finally separating the sedimented material.
  • the alkali water glass solutions and / or the polyalkylene glycol solutions are preferably preheated, in particular to 30 to 60 ° C., preferably to about 50 ° C.
  • An alternative method of operation is to heat in process stage (1) to a temperature of 60 to 80 ° C. in a closed agitator and, with intensive stirring, to add 0.5 to 2.5% by weight, based on the waste oil.
  • a hydrogenation treatment step known per se can be switched between process step (3) and process step (4), in which, in the presence of a hydrogenation-active catalyst, in particular at 200 to 400 ° C. and 10 to 200 105 Pa (10 to 200 bar ) and preferably at 300 to 380 ° C and 40 to 60 105 Pa (40 to 60 bar) the pretreated oil phase is hydrogenated.
  • a hydrogenation-active catalyst in particular at 200 to 400 ° C. and 10 to 200 105 Pa (10 to 200 bar ) and preferably at 300 to 380 ° C and 40 to 60 105 Pa (40 to 60 bar) the pretreated oil phase is hydrogenated.
  • the filter insert of process stage (4) or (8) is regenerated if necessary by washing it free of the adsorbed material with a solvent.
  • a ketone solvent is preferably used for this purpose, which in particular consists of one or more solvents each having a boiling point of 50 to 80 ° C. and is in particular acetone or methyl ethyl ketone.
  • the treated oil phase is finally subjected to vacuum distillation at a temperature of 200 to 300 ° C. and a pressure of 0.13 kPa to 6.67 kPa (1 to 50 torr).
  • a further embodiment of the process according to the invention provides for treatment of the dry oil phase (with water contents ⁇ 0.1% by weight) in a manner known per se after process step (3). with finely dispersed sodium.
  • Process steps (1) to (3) are able to deliver a constant water-free oil flow, which is the most important requirement for the use of sodium. Since the oxidation products and the non-PCB chlorine compounds are largely removed by the pretreatment in this water-free oil stream, the sodium process is economically viable.
  • the sodium required for the waste oil treatment is added to the pretreated waste oil in the form of a dispersion, in particular consisting of sodium particles of 5 to 10 ⁇ m, in a base oil of a similar composition to motor oils.
  • a dispersion in particular consisting of sodium particles of 5 to 10 ⁇ m, in a base oil of a similar composition to motor oils.
  • sodium in an oil, preferably reraffinate is melted and finely divided in a disperser, so that particle sizes of ⁇ 20 ⁇ m are achieved.
  • a dispersion of 33% by weight sodium is particularly suitable for the treatment of the pretreated dry oil stream.
  • the amount of dispersion added is matched to the content of inorganic chlorine.
  • the treatment temperature and time depend on the quality of the drying oil. Normally, a temperature range from 20 ° C to 250 ° C and especially in a temperature range from 100 to 200 ° C and in a period of 1 to 30 minutes reliable PCB separation can be achieved.
  • the base oil obtained is characterized by a cheaper and higher viscosity index than fresh oil. All ash-forming additives - otherwise the cause of sludge formation are removed, i.e. H. the ash content is practically 0% by weight. The viscosity improvement additives are largely retained, namely at least 1/3 of the corresponding additives in the fresh additive package.
  • Contaminants in waste oil form stable dispersions due to the presence of detergents. Additives prevent the physical separation of the contaminants by gravity and / or centrifugal force.
  • the flocculation and adsorbents namely alkali water glass and polyalkylene glycol of the formula given, destabilize the dispersion in process step (1). The differences in density between the oil and foreign matter phases are effective.
  • the chlorine compounds are chemically converted and NaCl and non-chlorinated compounds are formed. The oxidation products are neutralized and the converted and neutralized products are adsorbed.
  • process stage (2) impurities and the flocculants and adsorbents are separated off.
  • the flocculated, dispersed impurities are eliminated by decanters or separators as a result of the destabilization which took place in stage (1) and the density differences which became effective in stage (1) by the action of gravity or minimal centrifugal forces.
  • process stage (3) the low boilers, namely polar and non-polar solvents, and water are removed.
  • the solvent and adsorbent additive in process step (6) is used for the further precipitation of finely dispersed impurities, here these additives bring about the removal of polychlorinated bi- and terphenylene and the solvent additive supports the subsequent filtering adsorption step. If there are no polychlorinated bi- and terphenyls, the addition of the n-alkanes can be used to go directly to the filtering adsorption stage without the further addition of adsorbents - see process stage (4).
  • Process stage (6) with the addition of solvent and adsorbent is followed by process stage (7), which largely corresponds to process stage (2).
  • the filtering adsorption takes place in process stage (8) or (4). In this stage, the remaining dissolved and undissolved impurities and unwanted residual additives are specifically bound to the adsorbents.
  • the lubricating oil components (hydrocarbons) pass through the adsorbents.
  • This filtering adsorption is a multi-parameter separation method, which is characterized in that two chemically different substances or two chemically different groups of substances are separated from one another due to their different adsorption capacity, by allowing a specific solvent and an adsorbent to act on the mixture.
  • the filtering adsorption differs in that there is only a single phase during the separation, while the filtration requires two phases, generally solid / liquid.
  • the filtering adsorption distinguished by its selectivity, which is achieved by the selective solvent and a selected adsorbent, here bleaching earth or compacted aluminum oxide, see "Filtering adsorption", W. Fuchs, F. Glaser and E. Bendel, chemistry Engineering technology 1959, pages 677 679.
  • Adsorbed material namely 5 to 10% by weight of finely dispersed, dissolved oxidation products and residual additives, are desorbed with suitable solvents, solvents with a boiling point of up to 80 ° C., in particular acetone or methyl ethyl ketone.
  • the adsorbent is dried at about 60 to about 120 ° C., preferably about 100 ° C., under a protective gas, preferably nitrogen, and then brought to the temperature required for process step (8).
  • the adsorbent is now ready for use again and can be used continuously at these values.
  • the lubricating oil constituents (about 1.5% by weight) which are contained in the adsorbent are dissolved out before the adsorbent regeneration (with acetone or methyl ethyl ketone) by solvent rinsing, in particular with n-heptane, and fed to process stage (6) or (9).
  • This step serves to increase the yield of the regrind.
  • the residual additives and oxidation products obtained after evaporation of the solvent are used as additives, for example for asphalt processing.
  • PCBs, chlorinated dioxins, furans and aliphates with chlorine contents> 5% can be broken down below the detection limit in this way.
  • the recovered solvent is used again for solvent rinsing.
  • step (5) or (9) the solvent is separated from the regenerate and returned in step (4) or (6).
  • the final oil phase is a mixture of lubricating oil fractions with different flash points and viscosities, the fractions must be separated under vacuum and temperatures above 200 ° C.
  • the swamp is base oil.
  • the process comprising process steps (1) to (3) can be used for decentralized waste oil processing, in that the collected waste oils are brought together in area collection points and treated in decentralized small plants according to the process comprising process steps (1) to (3) as a partial process.
  • the waste oil treated in this way can then be subjected to the process according to one or more of the subclaims, in particular for the removal of chlorine compounds and perchlorinated bi- and terphenylene, in a central large-scale plant.
  • Adsorbent regeneration with acetone, methyl ethyl ketone (technical).
  • Filters used stainless steel, sieve mesh 20 ⁇ m to 200 ⁇ m; Glass fiber filter and non-woven filter.
  • the mixture obtained was sedimented in a decanter at 70 ° C with a throughput of 3,000 ml / h and the oil phase separated.
  • the low boilers and the residual water were separated from the oil phase at a temperature of 130 ° C. and a pressure of 6.67 kPa (50 torr).
  • Waste oil not containing PCBs was treated with n-heptane in the ratio of oil phase to n-heptane of 1: 4 parts by weight as a dry oil phase pretreated according to Example 1 in a closed agitator, and stirred intensively at 40 ° C. for 30 minutes.
  • the oil solution was then sedimented in a decanter at 10 to 20 ° C. with a throughput of 12,000 ml / h, and then the oil solution was separated from the precipitation residue.
  • PCB-containing waste oil was mixed in a closed agitator after the addition of n-heptane in the ratio oil phase to n-heptane of 1: 4 parts by weight to the oil phase pretreated according to Example 1 with intensive stirring at 80 ° C with a mixture of 0 preheated to 50 ° C , 25% by weight soda water glass 50/51 (alkaline) and 0.1% by weight of polyethylene glycol (average molecular weight 600, OH number 170 mgKOH / g), each based on the dry oil phase.
  • the mixture was stirred vigorously at 70 ° C. for about 110 minutes.
  • 0.1% by weight of anhydrous sodium metasilicate was added and the mixture was stirred for a further 10 minutes.
  • the oil solution was sedimented in a decanter at 10 to 20 ° C with a throughput of 12,000 ml / h and the oil solution was separated from the residue.
  • the oil solution from Examples 2 and 3 was subjected to a "filtering adsorption".
  • the adsorber consisted of a stainless steel screen mesh (20 - 40 ⁇ m) and an adsorbent pack with bleaching earth, Tonsil CCG 30/60.
  • the undesired oil components were adsorbed at 40 ° C. It was regenerated with n-heptane.
  • the throughput of regenerated solution was 3,000 ml / h.
  • the solvent n-heptane was recovered from the regenerated solution by distillation at 70 ° C. and a pressure of 6.67 kPa (50 torr).
  • the regenerate obtained was a mixture of lubricating oil fractions with different flash points and viscosities.
  • the fractions were separated under vacuum at 250-300 ° C and a pressure of before 0.13 kPa to 1.3 kPa (1 to 10 Torr).
  • the base oil was obtained as the sump.
  • the adsorber has been regenerated by desorbing the adsorbed impurities (oxidation products, unwanted residual additives, degradation products, etc.) at 50 ° C with acetone (boiling point 56 ° C).
  • the adsorber was dried under a stream of nitrogen at 60 ° C. and made reusable.
  • the resulting acetone solution was subjected to distillation to remove acetone from the waste.
  • the acetone was used again.
  • the wastes from Examples 1, 2, 3 and 4 were used as additives in the concentration range 0.5 to 5% by weight (based on bitumen) for asphalt modification.
  • process stage (4) instead of process stage (4) or (8), thin-film evaporation known per se can be carried out. Likewise, following the treatment with dispersed sodium, the oil phase obtained can be subjected to thin-film evaporation instead of process step (4).
  • the base oil obtained was characterized by a cheaper and higher viscosity index than the fresh oil. All ash-forming additives - otherwise causing sludge formation (especially in the engine) - are removed, ie the base oil obtained has an ash content of almost 0.0% by weight. Finally, the additives to improve the viscosity are largely retained, in accordance with previous ones Results at least about a third of the content of the fresh additive package in these additives.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Lubricants (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
EP88907226A 1987-08-19 1988-08-18 Verfahren zur reinigung und regenerierung von altölen Expired - Lifetime EP0377606B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88907226T ATE82769T1 (de) 1987-08-19 1988-08-18 Verfahren zur reinigung und regenerierung von altoelen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3727560 1987-08-19
DE3727560 1987-08-19

Publications (2)

Publication Number Publication Date
EP0377606A1 EP0377606A1 (de) 1990-07-18
EP0377606B1 true EP0377606B1 (de) 1992-11-25

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP88907226A Expired - Lifetime EP0377606B1 (de) 1987-08-19 1988-08-18 Verfahren zur reinigung und regenerierung von altölen

Country Status (8)

Country Link
US (1) US5141628A (el)
EP (1) EP0377606B1 (el)
JP (1) JPH02504523A (el)
CN (1) CN1021233C (el)
AU (1) AU2269788A (el)
DE (2) DE3876245D1 (el)
RU (1) RU1834902C (el)
WO (1) WO1989001508A1 (el)

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RU2600726C2 (ru) * 2014-12-15 2016-10-27 Федеральное государственное казенное военное образовательное учреждение высшего профессионального образования "Военная академия материально-технического обеспечения имени генерала армии А.В. Хрулёва" Министерства обороны Российской Федерации Способ регенерации отработанного масла
RU2614244C1 (ru) * 2016-05-30 2017-03-24 Федеральное государственное бюджетное научное учреждение "Всероссийский научно-исследовательский институт использования техники и нефтепродуктов в сельском хозяйстве" (ФГБНУ ВНИИТиН) Способ очистки отработанных минеральных моторных масел

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RU2717856C2 (ru) * 2016-11-15 2020-03-26 Алексей Сергеевич Курочкин Комплекс фильтров очистки диэлектрических жидкостей
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Publication number Priority date Publication date Assignee Title
RU2556221C1 (ru) * 2014-06-26 2015-07-10 Государственное научное учреждение Всероссийский научно-исследовательский институт использования техники и нефтепродуктов Российской академии сельскохозяйственных наук (ГНУ ВНИИТиН Россельхозакадемии) Способ регенерации отработанных синтетических моторных масел
RU2600726C2 (ru) * 2014-12-15 2016-10-27 Федеральное государственное казенное военное образовательное учреждение высшего профессионального образования "Военная академия материально-технического обеспечения имени генерала армии А.В. Хрулёва" Министерства обороны Российской Федерации Способ регенерации отработанного масла
RU2614244C1 (ru) * 2016-05-30 2017-03-24 Федеральное государственное бюджетное научное учреждение "Всероссийский научно-исследовательский институт использования техники и нефтепродуктов в сельском хозяйстве" (ФГБНУ ВНИИТиН) Способ очистки отработанных минеральных моторных масел

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US5141628A (en) 1992-08-25
CN1021233C (zh) 1993-06-16
DE3890632D2 (en) 1990-07-19
RU1834902C (ru) 1993-08-15
JPH02504523A (ja) 1990-12-20
DE3876245D1 (el) 1993-01-07
AU2269788A (en) 1989-03-09
WO1989001508A1 (en) 1989-02-23
CN1045122A (zh) 1990-09-05
EP0377606A1 (de) 1990-07-18

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