CN1107109C - Process for recovering waste oil - Google Patents

Process for recovering waste oil Download PDF

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Publication number
CN1107109C
CN1107109C CN 00123153 CN00123153A CN1107109C CN 1107109 C CN1107109 C CN 1107109C CN 00123153 CN00123153 CN 00123153 CN 00123153 A CN00123153 A CN 00123153A CN 1107109 C CN1107109 C CN 1107109C
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oil
recovery
bed hydrogenation
reaction
waste
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CN 00123153
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Chinese (zh)
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CN1351135A (en
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张忠清
张宏哲
董志学
贾丽
李鹤鸣
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中国石油化工股份有限公司
中国石油化工股份有限公司抚顺石油化工研究院
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Abstract

The present invention describes a combined technique method for recovering waste lubricating oil, which adopts a suspension bed hydrogenation technique process, and uses a high activity multiple metal water solubility catalyst to directly hydrogenize the waste oil. Product regenerating base oil and side product light oil are obtained by simple filtration, fixed bed hydrogenation refining, flash evaporation and product separation.

Description

A kind of recovery method of waste oil
The present invention relates to the recovery method of a kind of waste oil, particularly waste lubricating oil.
Along with people's environmental consciousness strengthen day by day and market to the increase of demand for lubricating oil, waste oil recycling paid more and more attention.The main purpose that waste oil reclaims is to produce the regeneration oil product, economizes on resources, protects environment.Thereby, be accompanied by each treatment process of waste oil processing and utilization, all have closely and get in touch with environment.
Recent years, increasing additive joins in the lubricating oil, for example: stain remover, pour point depressor, oxidation hold back agent and viscous modulus rising agent.These additives have improved the performance of lubricating oil greatly, and simultaneously, they have also increased the difficulty that reclaims waste lubricating oil.Particularly when adding the resin additive of standard state in the oil, except the metal impurities of carbon, mud, wearing and tearing, be suspended in the impurity in the engine oil in addition, for example: calcium and barium salt, ash free basis stain remover etc. by modern stain remover generation.Have only the various impurity of effectively removing in the waste oil, could reclaim and make lubricant base, reduce influence, produce qualified senior lubricant subsequent technique.
The PROP technology of US4151072 is joined together chemical demetalization and carclazyte/hydrotreatment purification step.At first, waste oil and water-soluble solvent (as the phosphoric acid diamine) mix, and this solvent and metallic impurity reaction generate corresponding metal salt, because the solubleness of this metal-salt in water and oil is little, just can separate them.Then, with the metal removal oil after the screen filtration heating, the carclazyte with the protection bed contacts again, then hydrogenation on the Ni/Mo catalyzer, washing at last.
The shortcoming of PROP technology is to produce a large amount of solid wastes in processing and filtration procedure, the waste carclazyte, and also this technology has generated the waste water that brought by chemical solvents in a large number.
US3919076, US4073719, US4073720 have introduced dehydration-de-oiling/solvent extraction/distillation/clay-filtered/hydrofining etc. respectively and have been used to handle the technological process of waste oil.In these technologies in order in the waste oil of dehydration/de-oiling, to reduce burnt and mud precursor, various extraction agents have been used, as: in the distillation front, remove with the mixture of propane or ethanol and ketone and to defocus and the mud precursor, the cut after the distillation carries out clay-filtered and hydrofining again.The shortcoming of these methods is solvent recovering system complexity, consume higher energy, and generates a large amount of chemical wastes.
US4512878 has announced that a kind of waste oil earlier through pre-treatment, removes impurity such as mud, and repeated hydrogenation is removed the combined technique of additive isopolarity compound.Concrete steps are: waste oil dewaters earlier/the de-oiling step; enter filtration unit then; remove the scrap metal that exists in gravel solid and the waste oil; enter water distilling apparatus then; the distillate that distillation is obtained is by containing the protection bed of active material again; remove phosphide and mud, select for use fixed bed to carry out hydrotreatment at last.
This technology preferably resolves the blockage problem of technological process; but in technological process in order to prevent to protect the blockage problem of bed and fixed-bed reactor; in distilation steps, need halogenide, phosphide and mud precursor are to the greatest extent at utmost removed; and do not stint the part useful component of carrying under one's arms out, thereby reduced product yield.
Existing patent and other disclosed waste oil treatment technology all do not have well to solve the blockage problem of base oil yield and hydrogenation unit.At present, it is simpler that a kind of technological process is actively sought in countries in the world, again can be in the technology of industrial easy realization.
The objective of the invention is to seek a kind of combination complete processing, this combination process can obtain the lube base oil product to greatest extent and produce lightweight oil and free from environmental pollution as far as possible less when processing waste oil.Another object of the present invention is to find a kind of technology that is suitable for handling various waste lubricating oils, and this technology can be handled various waste lubricating oils, and is applied widely, the product yield height.
For this reason, the present invention proposes a kind of combination treatment method of waste oil, i.e. the advanced floating bed hydrogenation device reaction of waste oil, hydrogenation is removed mud precursor, polar material etc., then after filtration, refining, the flash distillation of fixed bed hydrogenation, product separation obtain product.
Its concrete technological process is: (1), waste oil and catalyst mix, directly join in the suspension bed, and carry out hydrotreatment.(2), the hydrogenated oil that comes out from suspension bed remove through simple filtration deash, scrap metal etc.(3), filter oil enters fixed bed and carries out hydrofining and remove unsaturated hydro carbons.(4), the hydrogenated oil that comes out from fixed bed enters flashing tower and carries out product separation, obtains base oil product and light constituent.(5), light constituent enters product separator, isolates hydrogen and lightweight oil.
Wherein said suspension bed can adopt any existing suspension bed working method in the step (1).Catalyst system therefor used water dissolubility disperse type catalyzer, oil-soluble catalyst and/or other efficient disperse type catalyzer.Preferred water-soluble catalyst, containing metal Mo, Ni, W, Co etc. in the catalyzer, each set of dispense is than being Ni/Mo=0.01~0.5: 1, W/Mo=0~4: 1, Co/Mo=0~2: 1.At first catalyzer is scattered in the stock oil, the total add-on of catalyst metal is 50~800 μ g/g, is preferably 150~600 μ g/g.Contain and enter the floating bed hydrogenation reactor after the stock oil of catalyzer and hydrogen mix.Hydrogenation reaction takes place in waste oil in reactor, become low boiler cut in order to prevent waste oil hydrocracking.The suspension bed hydrogenation process condition is: reaction pressure is 3~11MPa, better is 4~6MPa; Temperature of reaction is 250~400 ℃, better is 300~360 ℃; The reaction solution hourly space velocity is 0.2~1.5h -1, be preferably 0.8~1.2h -1Hydrogen to oil volume ratio (under the standard pressure) is 100~1500, better is 300~800.
The material that comes out from suspended-bed reactor enter filtering system remove deash, impurity such as metal fragment.Filtering material can be diatomite, perlite and/or vegetable fibre, is preferably diatomite.Filtration temperature is 30~150 ℃, is preferably 60~120 ℃.
Enter fixed bed then and carry out hydrofining,, make the oil production of purification be fit to do lube stock to remove undersaturated alkene and remaining S, O, N etc.Hydrorefined processing condition and common raffinate hydrofining conditional likelihood, catalyzer can be common Hydrobon catalyst, and temperature of reaction is 250~400 ℃, better is 250~320 ℃; Hydrogen pressure is 3~11MPa, better is 4~6MPa; LHSV approximately is 0.5~4, better is 0.5~2; Gas speed is 1.5~15Kmol/m 3, better be 1.5~5Kmol/m 3
The hydrogenated oil that comes out from hydro-refining unit separates through flashing tower, obtains lubricating oil distillate at the bottom of the tower, and the lightweight oil and the hydrogen that flash off enter product separator.
Because during the waste oil hydrogenation, chlorine-containing compound wherein, sulfocompound can react and generate HCL and H 2S neutralizes so squeeze into aqueous sodium hydroxide solution in product separator, in order to avoid equipment corrosion.Lightweight oil separates at product separator with hydrogen, and hydrogen recycle is used.
Said waste oil can be waste vapour oil machine oil, waste diesel machine oil, useless industrial lubricant, useless electric insulation wet goods waste oil.
Below in conjunction with accompanying drawing a kind of scheme of the present invention is described in detail:
Fig. 1 is a kind of waste oil hydrotreatment process integration setting drawing of the present invention.
Wherein 1 is feed line, 2 is catalyst line, and 3 is mixing tank, and 4,6,7,9,11,13,14 is pipeline, 5 is pump, 8 is well heater, and 10 is the floating bed hydrogenation reactor, and 12 is high-pressure separator, 15 is strainer, 16 is fixed bed hydrogenation refining reaction device, and 17 is flashing tower, and 18 is product separator.
Its specific operation process is as follows:
Waste oil raw material and aqueous catalyst solution enter blender 3 from pipeline 1 and 2 respectively. Charging after mixing enters heater 8 through pipeline 4 and pump 5, pipeline 7, and hydrogen enters system via pipeline 6. Charging is heated to 150~200 ℃ in heating furnace 8, then enter reactor 10 through pipeline 9. Product enters high-pressure separator 12 via pipeline 11, tells gas and goes hydrofinishing fixed bed 16 to remove unsaturated hydro carbons through pipeline 14. High-pressure separator 12 isolated liquid materials go filtration system 15 to remove impurity through pipeline 13. Then enter fixed bed 16 and carry out hydrofinishing. Distill to flash column 17, get lube cut at the bottom of the tower, the light oil that flashes off and hydrogen enter product separator 18. Because during the waste oil hydrogenation, chlorine-containing compound wherein, sulfur-containing compound can react and generate HCL and H2S neutralizes so squeeze into sodium hydrate aqueous solution in product separator, in order to avoid equipment corrosion. Light oil separates at product separator with hydrogen, and hydrogen recycles.
Blender 3 wherein can be an agitator tank, also can be a colloid mill or static mixer or other conventional mixing apparatus, and waste oil and aqueous catalyst solution are mixed. If material viscosity is large especially, be difficult to use the conventional method mixing below 100 ℃, also can first aqueous catalyst solution be mixed with a small amount of waste oil, and then mix with full-bodied charging.
Advantage of the present invention is:
1. adopt the floating bed hydrogenation treatment process, there is not the bed blockage problem in this technology utilization suspension bed, thereby waste oil need pass through preliminary treatment, and the direct hydrogenation processing has significantly reduced production cost.
2. adopt the floating bed hydrogenation treatment process, can to greatest extent useful component be converted into lube base oil, product yield is high.
3. adopt the floating bed hydrogenation treatment process, raw material can be used oil, useless industrial lubricant, useless electric insulating oil, and raw material is applied widely.
4. the high activated catalyst that adopts can destroy additive molecule, mud precursor.
For further specifying all main points of the present invention, enumerate following examples.
Embodiment 1~3
Test raw material character sees Table 1.Carbon residue, acid number, oxidation stability numerical value height illustrate that the oxidation depth of oil is not shallow as shown in Table 1; Metal contents such as calcium, barium, magnesium, phosphorus, zinc are quite high, illustrate and contain a large amount of additives in the lubricating oil; Nitrogen in the oil and sulphur are from ash free basis additive and base oil; The iron level explanation corrosion to a certain degree and the existence of wearing and tearing.
Table 1 raw material waste vapour oil machine oil feedstock property
Project Numerical value Project Numerical value
Density (20 ℃), Kg/m 3 ????0.8888 ????H,% ????13.21
Flash-point (opening), ℃ ????228 ????S,% ????0.25
Ash content, % ????1.09 ????N,ppm ????1221
Neutralization value, mgKOH/g ????3.30 Metal analysis, ppm
Pour point, ℃ ????-30 ????Pb ????1276
Viscosity (100 ℃) ????16.44 ????Ca ????1855
<350 ℃ of cuts, w% ????11.2 ????Mg ????165.5
350~550 ℃ of cuts, w% ????65.3 ????Zn ????681.6
>550 ℃ of cuts, w% ????23.5 ????Mo ????19.87
Carbon residue, % ????3.77 ????Al ????12.86
150 ℃ of oxidation stabilities (rotary oxygen bomb method), min ????<120 ????Fe ????15.90
Ultimate analysis, % ????Na ????13.44
???C,% ????83.7
Waste oil hydrocracking situation under different condition is investigated in this test.At first prepare the aqueous catalyst solution that contains hydrogenation active metals, aqueous catalyst solution is joined carry out hydrogenation reaction in the waste oil then.
Process of the test is: take by weighing waste oil 200g and put into the autoclave that a 750mL band stirs, add a certain amount of catalyzer.Closed reactor, room temperature is filled hydrogen pressure to required pressure behind the logical hydrogen, begins then to stir to heat up, and reacts under required pressure.Make reactor keep constant pressure with the method for mending hydrogen continuously between the reaction period.Test-results sees Table 2
Table 2 suspension bed reaction conditions and hydrogenated oil character
Embodiment ????1 ????2 ????3
Reaction conditions
Temperature of reaction, ℃ ????360 ????330 ????300
Reaction pressure, MPa ????6 ????5 ????4
Reaction times, min ????45 ????60 ????80
The catalyzer add-on, μ g/g ????150 ????300 ????800
Hydrogenated oil character
Flash-point (opening), ℃ ????227 ????21.9 ????210
Ash content, w% ????0.46 ????0.76 ????0.5
Neutralization value, mgKOH/g ????0.98 ????1.23 ????1.08
Pour point, ℃ ????-8 ????-8 ????-10
Viscosity (100 ℃) ????10.73 ????12.54 ????13.07
<350 ℃ of cuts, w% ????12 ????11.3 ????11.4
350~550 ℃ of cuts, w% ????82.6 ????82.3 ????82.4
>550 ℃ of cuts, w% ????5.4 ????6.4 ????6.2
Carbon residue, w% ????0.47 ????0.58 ????0.79
Mechanical impurity, w% ????0.08 ????0.11 ????0.10
150 ℃ of 350~550 ℃ of cut oxidation stabilities (rotary oxygen bomb method), min ????79 ????87 ????120
????C,% ????84.48 ????84.01 ????83.73
????H,% ????12.73 ????12.64 ????12.54
????S,% ????0.24 ????0.24 ????0.24
????N,ppm ????1102 ????1083 ????978
The test-results explanation uses the floating bed hydrogenation process of multicomponent catalyst can significantly improve the quality of waste oil, and the nitrogen of hydrogenated oil, sulphur, carbon residue, ash content, mechanical impurity, oxidation stability obviously reduce; Pour point, flash-point, viscosity also have clear improvement.Lubricant base oil fraction can reach 82.6%, and yield of light oil is 12%, and total recovery is 94.6%.US4512878 narrates: yield of light oil is about 12%, 350~550 ℃ of cuts and is about 68% in removing the mud process, and residue is about 15%.Behind the normalizing, yield of light oil is about 12.63%, 350~550 ℃ of cuts and is about 71.6%, and residue is about 15.8%, well below yield of the present invention.
Embodiment 4~7
This test explanation reaction conditions still can obtain expected result when fluctuating in relative broad range.Reaction raw materials oil and process of the test are with embodiment 1~3, and test-results sees Table 3.
Waste oil hydropyrolysis experiment result under table 3 different technology conditions
Embodiment ????4 ????5 ????6 ????7
Temperature of reaction, ℃ ????260 ????260 ????380 ????380
Reaction pressure, MPa ????3 ????3 ????9 ????9
Reaction times, min ????60 ????60 ????50 ????50
The catalyzer add-on, μ g/g ????100 ????100 ????800 ????800
Flash-point (opening), ℃ ????217 ????219 ????210 ????216
Ash content, w% ????0.66 ????0.79 ????0.53 ????0.6
Neutralization value, mgKOH/g ????1.38 ????1.23 ????1.08 ????1.09
Pour point, ℃ ????-9 ????-8 ????-10 ????-11
Viscosity (100 ℃) ????11.73 ????12.94 ????12.07 ????11.98
Carbon residue, w% ????0.68 ????0.76 ????0.83 ????0.89
Mechanical impurity, w% ????0.09 ????0.13 ????0.12 ????0.1
150 ℃ of 350~550 ℃ of cut oxidation stabilities (rotary oxygen bomb method), min ????86 ????83 ????81 ????73
Embodiment 8~9
The result of the waste oil hydrotreatment combined process that this test explanation is carried out on continuous apparatus.
Fig. 1 is seen in the signal of waste oil hydrotreatment process integration continuous apparatus flow process.Waste oil raw material and aqueous catalyst solution enter mixing tank 3 from pipeline 1 and 2 respectively.Charging after mixing enters well heater 8 through pipeline 4 and pump 5, pipeline 7, and hydrogen enters system via pipeline 6.Charging is heated to 170 ℃ in process furnace 8, enter reactor 10 through pipeline 9 then.Reaction product enters high-pressure separator 12 via pipeline 11, tells gas and goes hydrofining fixed bed 16 to remove unsaturated hydro carbons through pipeline 14.High-pressure separator 12 isolated liquid materials go filtering system 15 to remove impurity through pipeline 13.Enter fixed bed 16 then and carry out hydrofining.Distill to flashing tower 17, get lubricating oil distillate at the bottom of the tower, light oil that flashes off and hydrogen enter product separator 18.Operation condition and test-results see Table 4.
Table 4 reaction conditions and product oil properties
Embodiment HVI base oil standard ????8 ????9
Reaction conditions
The suspension bed temperature of reaction, ℃ ????300 ????350
The suspension bed reaction pressure, MPa ????4 ????6
The suspension bed hydrogen to oil volume ratio ????300 ????1000
The strainer filtration temperature, ℃ ????60 ????120
The fixed bed reaction temperature, ℃ ????260 ????320
Fixed bed reaction pressure, MPa ????3 ????5
Fixed bed LHSV ????0.5 ????2
Fixed bed gas speed Kmol/m 3 ????1.5 ????5
The product oil nature
Flash-point (opening), ℃ ????>175 ????221 ????217
Ash content, % ????0.01 ????0.01
Neutralization value, mgKOH/g ????<0.02 ????<0.04 ????<0.04
Pour point, ℃ ????<-9 ????-15 ????-20
Viscosity (100 ℃) Report * ????5.03 ????5.05
<350 ℃ of cuts, w% ????12.3 ????12.4
350~550 ℃ of cuts, w% ????85.3 ????85.0
>550 ℃ of cuts, w% ????2.4 ????2.6
Carbon residue % ????<0.25 ????<0.25 ????<0.25
Mechanical impurity, % Do not have Do not have
150 ℃ of 350~550 ℃ of cut oxidation stabilities (rotary oxygen bomb method), min ????>180 ????200 ????185
??S,% Report * ????0.01 ????0.01
??N,ppm Report * ????675 ????542
Annotate: * refers to that this index do not do requirement.
The test-results explanation, waste oil all drops to prescribed value through ash content, carbon residue, the mechanical impurity that floating bed hydrogenation is handled, strainer filters back end hydrogenation oil.After fixed bed hydrogenation is refining, removed unsaturated hydro carbons, the oxidation stability numerical value of product oil reaches prescribed value, and the product oil nature reaches HVI base oil standard.The base oil yield that<350 ℃ yield of light oil is about 12.3%, 350~550 ℃ of cuts is about 85.3%, and total recovery reaches 97.3%.

Claims (10)

1. the recovery method of a waste oil is characterized in that the advanced floating bed hydrogenation device of waste oil, carries out hydrotreatment in the presence of hydrogen and suspension bed hydrogenation catalyst, then after filtration, fixed bed hydrogenation makes with extra care, flash distillation, product separation obtain product; Wherein said suspension bed hydrogenation process condition is: reaction pressure is 3~11MPa, and temperature of reaction is 250~400 ℃, and the reaction solution hourly space velocity is 0.2~1.5h -1, hydrogen to oil volume ratio is 100~1500; Described fixed bed hydrogenation process for refining condition is: temperature of reaction is 250~400 ℃, and hydrogen pressure is 3~11MPa, and volume space velocity is 0.5~4h -1, gas speed is 1.5~15Kmol/m 3
2. according to the described recovery method of claim 1, wherein said suspension bed hydrogenation catalyst is water-soluble catalyst, oil-soluble catalyst and/or other disperse type catalyzer.
3. according to the described recovery method of claim 1, wherein said suspension bed hydrogenation catalyst is a water-soluble catalyst, containing metal Mo, Ni, W, Co in the catalyzer, and each set of dispense is than being Ni/Mo=0.01~0.5: 1, W/Mo=0~4: 1, Co/Mo=0~2: 1.
4. according to the described recovery method of claim 1, wherein said suspension bed hydrogenation catalyst is 50~800 μ g/g in the metal add-on.
5. according to the described recovery method of claim 4, wherein said suspension bed hydrogenation catalyst is 150~600 μ g/g in the metal add-on.
6. according to the described recovery method of claim 1, wherein said suspension bed hydrogenation process condition is: reaction pressure is 4~6MPa; Temperature of reaction is 300~360 ℃; The reaction solution hourly space velocity is 0.8~1.2h -1Hydrogen to oil volume ratio is 300~800.
7. according to the described recovery method of claim 1, used material is diatomite, perlite and/or vegetable fibre in the wherein said filtration, and filtration temperature is 30~150 ℃.
8. according to the described recovery method of claim 1, material therefor is a diatomite in the wherein said filtration, and filtration temperature is 60~120 ℃.
9. according to the described recovery method of claim 1, wherein said hydrorefined temperature of reaction is 250~320 ℃; Hydrogen pressure is 4~6MPa; Volume space velocity is 0.5~2h -1Gas speed is 1.5~5Kmol/m 3
10. according to the described recovery method of claim 1, wherein said waste oil is waste vapour oil machine oil, waste diesel machine oil, useless industrial lubricant, useless electric insulating oil.
CN 00123153 2000-10-26 2000-10-26 Process for recovering waste oil CN1107109C (en)

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US8088276B2 (en) 2008-08-08 2012-01-03 CleanOil Limited Oil re-refining system and method

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CN100334189C (en) * 2003-04-26 2007-08-29 荆门石油化工设计院 Technique for regenerating waste lubricating oil
ES2199697B1 (en) * 2003-09-23 2005-02-01 Sener Grupo De Ingenieria, S.A. PROCEDURE FOR REGENERATING OILS USED BY DEMETALIZATION AND DISTILLATION.
CN101173202B (en) * 2006-11-01 2010-09-15 中国石油化工股份有限公司 Waste lubricant oil recovery utilization method
CN102408942B (en) * 2011-10-20 2013-12-04 烟台易斯特机械制造有限公司 Device and preparation method for hydrorefining basic oil from waste internal-combustion engine oil
CN102776020A (en) * 2012-08-08 2012-11-14 赵世洲 Safe and environment-friendly oil refining process and device
CN104178210B (en) * 2013-05-27 2018-08-03 山东恒利热载体工程技术有限公司 The method and process unit of higher boiling conduction oil are discarded in a kind of recycling
CN104611007B (en) * 2015-02-25 2016-05-11 烟台荣盛压力容器制造有限公司 A kind of waste lubricating oil refines petrol and diesel oil device
CN104927918B (en) * 2015-06-12 2016-12-07 中国石油大学(华东) A kind of waste lubricating oil produces the combination regeneration method of top-grade lubricating oil product
CN106147857B (en) * 2016-08-19 2018-11-20 广州恒滤环保科技有限公司 A kind of environmentally friendly internal combustion engine used oil recycling technique
CN107325839A (en) * 2017-07-12 2017-11-07 宁波中循环保科技有限公司 Method for regenerating waste lubricating oil
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CN109468163B (en) * 2018-04-13 2021-04-16 湖北爱国石化有限公司 Refining process for waste mineral raw oil
CN110194968B (en) * 2019-04-30 2021-02-19 武汉金中石化工程有限公司 Waste lubricating oil full-component suspension bed hydrogenation regeneration process

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US8088276B2 (en) 2008-08-08 2012-01-03 CleanOil Limited Oil re-refining system and method

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