CN102732369A - Regeneration process for waste lubricating oil - Google Patents
Regeneration process for waste lubricating oil Download PDFInfo
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- CN102732369A CN102732369A CN2011102011115A CN201110201111A CN102732369A CN 102732369 A CN102732369 A CN 102732369A CN 2011102011115 A CN2011102011115 A CN 2011102011115A CN 201110201111 A CN201110201111 A CN 201110201111A CN 102732369 A CN102732369 A CN 102732369A
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Abstract
The invention discloses a regeneration process for waste lubricating oil. The process mainly comprises the procedures of deposition, distillation, pickling, adsorption with white clay and filtering and is characterized in that 2 to 4 parts by weight of No. 120 solvent naphtha is added into every 100 parts by weight of waste lubricating oil before pickling so as to realize dilution, then the procedures of pickling and adsorption with white clay are carried out and underpressure distillation is simultaneously carried out as adsorption with white clay is carried out so as to remove the No. 120 solvent naphtha through distillation. According to the invention, a diluent is added into waste lubricating oil for dilution to reduce viscosity of lubricating oil, which enables refining temperature to drop to an appropriate range, usage amount of sulfuric acid to be effectively reduced, pickling effects to be improved, usage amount of white clay to be reduced at the same time, regeneration cost to be substantially decreased and refining quality to be enhanced; and the diluent can be recycled, thereby effectively saving resources and further reducing pollution to the environment.
Description
Technical field
The present invention relates to a kind of process of regenerating of waste lubricating oil.
Background technology
At present, along with the minimizing day by day of petroleum resources and the continuous increase of demand, oil price is risen steadily; The recycling of waste lubricating oil not only can reduce environmental pollution, can also effectively economize on resources, therefore; It is particularly important that the recycling of waste lubricating oil also seems; Acid-white-clay type treatment process is often adopted in the regeneration of lubricating oil, and this process for purification has less investment, characteristics that flexibility property is strong, is well suited for middle-size and small-size lubricant oil regeneration enterprise and uses; It is wider also to meet the waste lubricating oil distribution, and a lot of lubricant oil regeneration enterprises all are the characteristics of medium and small sized enterprises.
In traditional acid-clay-filtered technology, at first be the acid treating of carrying out waste lubricating oil, the factor that influences acid treating has: the viscosity of vitriolic concentration, waste lubricating oil and extraction temperature, under the certain situation of sulfuric acid concentration; Viscosity and purified temperature by waste lubricating oil decide the vitriolic consumption jointly, and the viscosity and the temperature of waste lubricating oil are inversely proportional to, and temperature HV more is low more, and temperature LV more is high more; If extraction temperature is low excessively, oil body is just big, and sulfuric acid contacts insufficient with lubricating oil; Reaction is incomplete, the necessary increasing vitriolic consumption of making use of momentum like this, and this has also caused the sulfuric acid of not participating in reaction to discharge with acid sludge; Cause unnecessary waste, also polluted environment, simultaneously; The excessive sedimentation to acid sludge of oil body has also brought certain difficulty, if the temperature of sulfuric acid treatment is too high, sulfuric acid reaction is violent; The acid sludge that generates is just many, and side reaction simultaneously increases, and sulfuric acid can generate sulfonic acid with the effective constituent reaction in the waste lubricating oil; These sulfonic acid parts are along with acid sludge sedimentation together, and another part is dissolved in the sour oil, and prior art is difficult in the subsequent technique and removes; Influence the refining of lubricating oils quality, the bad usage quantity that has also strengthened carclazyte in the clay-filtered operation of pickling quality has also caused certain environmental pollution.
Introduced the method for sulfuric acid-clay-filtered rerefined oil in 2004 editions " waste lubricant oil regeneration " (petroleum industry press) book in detail: elder generation is mixed with waste lubricating oil with the form of spraying with 98% the vitriol oil; Utilize the effect such as deoxidation, desulfurization, degreasing, sulfonation, dissolving of the vitriol oil; With oxide compound, sulfide, the colloid of waste lubricating oil, effect such as bituminous matter forms acid sludge, long-time then sedimentation; Repeatedly divide the method for slag acid sludge to be removed clean; Adopt the method for carclazyte absorption at last, the sour oil behind minute slag is adsorbed, to remove sulfuric acid wherein.
For the waste lubricating oil that is mixed with light fuels such as gasoline, kerosene, diesel oil, Shao Min etc. are at " supercritical fluid extraction fractionation regeneration waste lubricating oil technology " ([J]; Refining of petroleum and chemical industry: 1997 10 phases) introduced a kind of renovation process of air distillation in the literary composition.In order to reduce distillation temperature, adopted when distillation and in oil, be blown into water vapour, through the rolling action of water vapour,, under the temperature that is lower than their boiling points, steam with gasoline, kerosene, diesel oil and light lubricating oil cut, heavy grease is stayed base product.
Above-mentioned process method still exist the usage quantity usage quantity of sulfuric acid, carclazyte etc. too high cause waste and pollute big and the temperature refining temperature higher, the deficiency that the refining quality is lower.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that exists in the present acid-clay-filtered lubricating oil technology, and a kind of process method of waste lubricant oil regeneration is provided, and can make extraction temperature further be reduced to suitable scope; And then can reduce the vitriolic usage quantity effectively; Improve pickling effectiveness, also can reduce the carclazyte usage quantity simultaneously, reduce regeneration cost greatly; Improve the refining quality; And all right recycling of described thinner economizes on resources effectively, and then reduces the pollution to environment.
In order to solve the problems of the technologies described above; The technical scheme that the present invention adopts is: comprise deposition, distillation, pickling, carclazyte absorption and filter operation; It is characterized in that: the 120# solvent oil that adds 2～4 weight parts in the waste lubricating oil by per 100 weight parts before described pickling dilutes; Get into pickling and carclazyte absorbing process afterwards, and when carrying out carclazyte absorption, carry out underpressure distillation, distill out the 120# solvent oil.
As the improvement of technique scheme, said underpressure distillation operation is preferably distilled through vacuumizing in the decompression and feeding 120～140 ℃ water vapour in still kettle.
As further improvement, the adding of carclazyte preferably is transported in the still kettle through the method that vacuumizes the decompression suction in the above-mentioned carclazyte absorbing process, and add-on is 3～5 weight parts.
As optimized technical scheme, the vitriol oil concentration in the above-mentioned pickling is preferably 93%～98%, and consumption is 1～3 weight part.
As preferred scheme, above-mentioned pickling is preferably under 20～30 ℃ of temperature to be carried out.
The present invention dilutes through in waste lubricating oil, adding thinner, reduces oil body, can make extraction temperature be reduced to suitable scope; Can reduce the vitriolic usage quantity effectively, improve pickling effectiveness, also can reduce the carclazyte usage quantity simultaneously; Reduce regeneration cost greatly, improve the refining quality, and all right recycling of described thinner; Economize on resources effectively, and then reduce pollution environment.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.
Fig. 1 is the process flow diagram of the embodiment of the invention 1.
Among the figure: 1 is waste lubricating oil, and 2 is water and particulate contamination, and 3 is pressurized air, and 4 is water and insoluble impurities, and 5 is light-weight fuel oil; 6 is thinner, and 7 is the vitriol oil, and 8 is high-pressure air, and 9 is acid sludge; 10 is overheated steam, and 11 is carclazyte, 12 thinners for recovery, and 13 is processed oil.
Embodiment
Embodiment 1: with reference to attachingFigure is the process flow diagram of the embodiment of the invention 1, and waste lubricating oil 1 is poured in the settling tank through classification; Remove wherein portion water and particulate contamination 2 through the natural sedimentation more than 24 hours, then raw oil is joined in the slurry tank, be heated to 60～80 ℃; Add emulsion splitter polyoxyethylene polyoxypropylene alkyl ethoxylated 0.2～0.4 weight part, flocculation agent SEPIGEL 305 0.05～0.15 weight part by per 100 weight part waste lubricating oils, feed pressurized air 3 simultaneously and stir, stir after 20～40 minutes; Standing sedimentation 4～6 hours, drainage water and insoluble impurities 4, lubricating oil after the sedimentation is heated to 260～270 ℃ through process furnace and enters into distillation tower and distill; Steam light-weight fuel oil 5 wherein, the lubricating oil after the distillation enters into pickling tank after being cooled to 20～30 ℃ through interchanger, adds thinner 6 120# solvent oils 2～4 weight parts by the lubricating oil after the above-mentioned distillation of per 100 weight parts; Feed high-pressure air 8 simultaneously and stir, add the vitriol oil 7 of 1～3 weight part 93%～98% afterwards, controlled temperature is at 20～30 ℃; Continue to stir 40～50 minutes, left standstill 6～8 hours, discharge acid sludge 9; Then lubricating oil is entered into still kettle, the top through still kettle vacuumizes the formation negative pressure, sucks the carclazyte 11 of 3～5 weight parts again through another pipeline through negative pressure; Stir simultaneously; Feed 120～140 ℃ overheated steam 10 after stirring and vacuumize underpressure distillation, distill out thinner, the thinner 12 of thinner through obtaining reclaiming after the alkaline purification; Can recycle; The lubricating oil of band carclazyte is cooled to 80～100 ℃ through interchanger again in the still kettle, is adjusted to neutrality through filtering the back with quadrol or NaOH again, can obtain processed oil 13.
Embodiment 2:With waste lubricating oil in settling tank through entering into slurry tank after 24 hours the natural sedimentation, in slurry tank, be heated to 60 ℃, add the emulsion splitter polyoxyethylene polyoxypropylene alkyl ethoxylated of 0.4 weight part and the flocculation agent SEPIGEL 305 of 0.15 weight part by per 100 weight part waste lubricating oils; Feed pressurized air simultaneously and stir after 40 minutes standing sedimentation 6 hours, drainage water and impurity; Lubricating oil after the sedimentation is heated to 260 ℃ through process furnace and enters into distillation tower and distill, and steams light-weight fuel oil wherein, and the lubricating oil after the distillation enters into pickling tank after being cooled to 20 ℃ through interchanger; The 120# solvent oil that adds 4 weight parts by the lubricating oil after the above-mentioned distillation of per 100 weight parts dilutes, and feeds high-pressure air simultaneously and stirs, and adds the vitriol oil of 1 weight part 98% again; Controlled temperature continues to stir 40 minutes at 20 ℃, leaves standstill 6 hours; Discharge acid sludge, get into then in the still kettle, the top through still kettle vacuumizes; In still kettle, form negative pressure, suck the carclazyte of 3 weight parts again through negative pressure, carry out mechanical stirring simultaneously; The overheated steam that feeds 140 ℃ after stirring distills, and distills out thinner, and thinner can recycle through alkaline purification; The lubricating oil of band carclazyte is cooled to 80 ℃ through interchanger again in the still kettle, filters through flame filter press again, removes carclazyte wherein; Be adjusted to neutrality with quadrol, can obtain processed oil.
Embodiment 3:With the waste lubricating oil that reclaims in settling tank through entering into slurry tank after 30 hours the natural sedimentation, in slurry tank, be heated to 63 ℃, add the emulsion splitter polyoxyethylene polyoxypropylene alkyl ethoxylated of 0.35 weight part and the flocculation agent SEPIGEL 305 of 0.13 weight part by per 100 weight part waste lubricating oils; Feed pressurized air simultaneously and stir after 35 minutes standing sedimentation 5.5 hours, drainage water and impurity; Lubricating oil after the sedimentation is heated to 263 ℃ through process furnace and enters into distillation tower and distill, and steams light-weight fuel oil wherein, and the lubricating oil after the distillation enters into pickling tank after being cooled to 23 ℃ through interchanger; The 120# solvent oil that adds 3.5 weight parts by the lubricating oil after the above-mentioned distillation of per 100 weight parts dilutes, and feeds high-pressure air simultaneously and stirs, and adds the vitriol oil of 1.5 weight parts 96% again; Controlled temperature continues to stir 42 minutes at 23 ℃, leaves standstill 6.5 hours; Discharge acid sludge, get into then in the still kettle, the top through still kettle vacuumizes; In still kettle, form negative pressure, suck the carclazyte of 3.5 weight parts again through negative pressure, carry out mechanical stirring simultaneously; The overheated steam that feeds 135 ℃ after stirring distills, and distills out thinner, and thinner can recycle through alkaline purification; The lubricating oil of band carclazyte is cooled to 85 ℃ through interchanger again in the still kettle, filters through flame filter press again, removes carclazyte wherein; Be adjusted to neutrality with quadrol, can obtain processed oil.
Embodiment 4:With the waste lubricating oil that reclaims in settling tank through entering into slurry tank after 36 hours the natural sedimentation, in slurry tank, be heated to 70 ℃, add the emulsion splitter polyoxyethylene polyoxypropylene alkyl ethoxylated of 0.3 weight part and the flocculation agent SEPIGEL 305 of 0.1 weight part by per 100 weight part waste lubricating oils; Feed pressurized air simultaneously and stir after 30 minutes standing sedimentation 5 hours, drainage water and impurity; Lubricating oil after the sedimentation is heated to 265 ℃ through process furnace and enters into distillation tower and distill, and steams light-weight fuel oil wherein, and the lubricating oil after the distillation enters into pickling tank after being cooled to 25 ℃ through interchanger; The 120# solvent oil that adds 3 weight parts by the lubricating oil after the above-mentioned distillation of per 100 weight parts dilutes, and feeds high-pressure air simultaneously and stirs, and adds the vitriol oil of 2 weight parts 95% again; Controlled temperature continues to stir 45 minutes at 25 ℃, leaves standstill 7 hours; Discharge acid sludge, get into then in the still kettle, the top through still kettle vacuumizes; In still kettle, form negative pressure, suck the carclazyte of 4 weight parts again through negative pressure, carry out mechanical stirring simultaneously; The overheated steam that feeds 130 ℃ after stirring distills, and distills out thinner, and thinner can recycle through alkaline purification; The lubricating oil of band carclazyte is cooled to 90 ℃ through interchanger again in the still kettle, filters through flame filter press again, removes carclazyte wherein; Be adjusted to neutrality with quadrol, can obtain processed oil.
Embodiment 5:With reclaim waste lubricating oil in settling tank through entering into slurry tank after 40 hours the natural sedimentation, in slurry tank, be heated to 72 ℃, add the emulsion splitter polyoxyethylene polyoxypropylene alkyl ethoxylated of 0.25 weight part and the flocculation agent SEPIGEL 305 of 0.08 weight part by per 100 weight part waste lubricating oils; Feed pressurized air simultaneously and stir after 25 minutes standing sedimentation 4.5 hours, drainage water and impurity; Lubricating oil after the sedimentation is heated to 268 ℃ through process furnace and enters into distillation tower and distill, and steams light-weight fuel oil wherein, and the lubricating oil after the distillation enters into pickling tank after being cooled to 27 ℃ through interchanger; The 120# solvent oil that adds 2.5 weight parts by the lubricating oil after the above-mentioned distillation of per 100 weight parts dilutes, and feeds high-pressure air simultaneously and stirs, and adds the vitriol oil of 2.5 weight parts 94% again; Controlled temperature continues to stir 47 minutes at 27 ℃, leaves standstill 7.5 hours; Discharge acid sludge, get into then in the still kettle, the top through still kettle vacuumizes; In still kettle, form negative pressure, suck the carclazyte of 4.5 weight parts again through negative pressure, carry out mechanical stirring simultaneously; The overheated steam that feeds 125 ℃ after stirring distills, and distills out thinner, and thinner can recycle through alkaline purification; The lubricating oil of band carclazyte is cooled to 95 ℃ through interchanger again in the still kettle, filters through flame filter press again, removes carclazyte wherein; Be adjusted to neutrality with quadrol, can obtain processed oil.
Embodiment 6:With reclaim waste lubricating oil in settling tank through entering into slurry tank after 48 hours the natural sedimentation, in slurry tank, be heated to 80 ℃, add the emulsion splitter polyoxyethylene polyoxypropylene alkyl ethoxylated of 0.2 weight part and the flocculation agent SEPIGEL 305 of 0.05 weight part by per 100 weight part waste lubricating oils; Feed pressurized air simultaneously and stir after 20 minutes standing sedimentation 4 hours, drainage water and impurity; Lubricating oil after the sedimentation is heated to 270 ℃ through process furnace and enters into distillation tower and distill, and steams light-weight fuel oil wherein, and the lubricating oil after the distillation enters into pickling tank after being cooled to 30 ℃ through interchanger; The 120# solvent oil that adds 2 weight parts by the lubricating oil after the above-mentioned distillation of per 100 weight parts dilutes, and feeds high-pressure air simultaneously and stirs, and adds the vitriol oil of 3 weight parts 93% again; Controlled temperature continues to stir 50 minutes at 30 ℃, leaves standstill 8 hours; Discharge acid sludge, get into then in the still kettle, the top through still kettle vacuumizes; In still kettle, form negative pressure, suck the carclazyte of 5 weight parts again through negative pressure, carry out mechanical stirring simultaneously; The overheated steam that feeds 120 ℃ after stirring distills, and distills out thinner, and thinner can recycle through alkaline purification; The lubricating oil of band carclazyte is cooled to 100 ℃ through interchanger again in the still kettle, filters through flame filter press again, removes carclazyte wherein; Be adjusted to neutrality with quadrol, can obtain processed oil.
Embodiment 7:With the waste lubricating oil that reclaims in settling tank through entering into slurry tank after 48 hours the natural sedimentation, in slurry tank, be heated to 75 ℃, add the emulsion splitter polyoxyethylene polyoxypropylene alkyl ethoxylated of 0.35 weight part and the flocculation agent SEPIGEL 305 of 0.1 weight part by per 100 weight part waste lubricating oils; Feed pressurized air simultaneously and stir after 60 minutes standing sedimentation 12 hours, drainage water and impurity; Lubricating oil after the sedimentation is heated to 260 ℃ through process furnace and enters into distillation tower and distill, and steams light-weight fuel oil wherein, and the lubricating oil after the distillation enters into pickling tank after being cooled to 28 ℃ through interchanger; The 120# solvent oil that adds 3.5 weight parts by the lubricating oil after the above-mentioned distillation of per 100 weight parts dilutes, and feeds high-pressure air simultaneously and stirs, and adds the vitriol oil of 1 weight part 98% again; Controlled temperature continues to stir 40 minutes at 20 ℃, leaves standstill 6 hours; Discharge acid sludge, get into then in the still kettle, the top through still kettle vacuumizes; In still kettle, form negative pressure, suck the carclazyte of 3 weight parts again through negative pressure, carry out mechanical stirring simultaneously; The overheated steam that feeds 140 ℃ after stirring distills, and distills out thinner, and thinner can recycle through alkaline purification; The lubricating oil of band carclazyte is cooled to 80 ℃ through interchanger again in the still kettle, filters through flame filter press again, removes carclazyte wherein; Be adjusted to neutrality with quadrol, can obtain processed oil.
Embodiment 8:With the waste lubricating oil that reclaims in settling tank through entering into slurry tank after 18 hours the natural sedimentation, in slurry tank, be heated to 65 ℃, add the emulsion splitter polyoxyethylene polyoxypropylene alkyl ethoxylated of 0.3 weight part and the flocculation agent SEPIGEL 305 of 0.18 weight part by per 100 weight part waste lubricating oils; Feed pressurized air simultaneously and stir after 45 minutes standing sedimentation 8 hours, drainage water and impurity; Lubricating oil after the sedimentation is heated to 263 ℃ through process furnace and enters into distillation tower and distill, and steams light-weight fuel oil wherein, and the lubricating oil after the distillation enters into pickling tank after being cooled to 23 ℃ through interchanger; The 120# solvent oil that adds 2.5 weight parts by the lubricating oil after the above-mentioned distillation of per 100 weight parts dilutes, and feeds high-pressure air simultaneously and stirs, and adds the vitriol oil of 1.5 weight parts 96% again; Controlled temperature continues to stir 30 minutes at 25 ℃, leaves standstill 6 hours; Discharge acid sludge, get into then in the still kettle, the top through still kettle vacuumizes; In still kettle, form negative pressure, suck the carclazyte of 2.5 weight parts again through negative pressure, carry out mechanical stirring simultaneously; The overheated steam that feeds 135 ℃ after stirring distills, and distills out thinner, and thinner can recycle through alkaline purification; The lubricating oil of band carclazyte is cooled to 85 ℃ through interchanger again in the still kettle, filters through flame filter press again, removes carclazyte wherein; Be adjusted to neutrality with quadrol, can obtain processed oil.
Claims (9)
1. the process method of a waste lubricant oil regeneration; Comprise deposition, distillation, pickling, carclazyte absorption and filter operation; It is characterized in that: the 120# solvent oil that adds 2～4 weight parts in the waste lubricating oil by per 100 weight parts before described pickling dilutes; Get into pickling and carclazyte absorbing process afterwards, and when carrying out carclazyte absorption, carry out underpressure distillation, distill out the 120# solvent oil.
2. the process method of waste lubricant oil regeneration according to claim 1 is characterized in that: said underpressure distillation is in still kettle, to carry out through vacuumizing in the decompression and feeding 120～140 ℃ water vapour.
3. the process method of waste lubricant oil regeneration according to claim 1 and 2 is characterized in that: the adding of carclazyte is transported in the still kettle through the method that vacuumizes decompression and suck in the described carclazyte absorbing process, and add-on is 3～5 weight parts.
4. the process method of waste lubricant oil regeneration according to claim 1 and 2, it is characterized in that: the vitriol oil concentration of said pickling is 93%～98%, consumption is 1～3 weight part.
5. the process method of waste lubricant oil regeneration according to claim 3, it is characterized in that: the vitriol oil concentration of said pickling is 93%～98%, consumption is 1～3 weight part.
6. the process method of waste lubricant oil regeneration according to claim 1 and 2, it is characterized in that: said pickling is carried out under 20～30 ℃.
7. the process method of waste lubricant oil regeneration according to claim 3, it is characterized in that: said pickling is carried out under 20～30 ℃.
8. the process method of waste lubricant oil regeneration according to claim 4, it is characterized in that: said pickling is carried out under 20～30 ℃.
9. the process method of waste lubricant oil regeneration according to claim 5, it is characterized in that: said pickling is carried out under 20～30 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104745285A (en) * | 2015-04-16 | 2015-07-01 | 中科院广州能源所盱眙凹土研发中心 | Regeneration method for waste lubrication oil |
| CN109652195A (en) * | 2018-11-14 | 2019-04-19 | 山东源根石油化工有限公司 | A kind of method for purifying and recovering of lubricating oil |
| CN110088257A (en) * | 2016-12-20 | 2019-08-02 | 阿法拉伐股份有限公司 | Pollutant is from the separation in liquid mixture |
| CN110207017A (en) * | 2019-07-03 | 2019-09-06 | 上海赛科石油化工有限责任公司 | A kind of spent solvent exhaust system and application thereof |
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| US3639229A (en) * | 1970-06-29 | 1972-02-01 | Exxon Research Engineering Co | Refining of used lubricating oils |
| CN1539936A (en) * | 2003-04-26 | 2004-10-27 | 荆门石油化工设计院 | Technique for regenerating waste lubricating oil |
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| US3639229A (en) * | 1970-06-29 | 1972-02-01 | Exxon Research Engineering Co | Refining of used lubricating oils |
| CN1539936A (en) * | 2003-04-26 | 2004-10-27 | 荆门石油化工设计院 | Technique for regenerating waste lubricating oil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104745285A (en) * | 2015-04-16 | 2015-07-01 | 中科院广州能源所盱眙凹土研发中心 | Regeneration method for waste lubrication oil |
| CN104745285B (en) * | 2015-04-16 | 2018-04-13 | 中科院广州能源所盱眙凹土研发中心 | Method for regenerating waste lubricating oil |
| CN110088257A (en) * | 2016-12-20 | 2019-08-02 | 阿法拉伐股份有限公司 | Pollutant is from the separation in liquid mixture |
| US11104863B2 (en) | 2016-12-20 | 2021-08-31 | Alfa Laval Corporate Ab | Separation of contaminants from a liquid mixture |
| CN109652195A (en) * | 2018-11-14 | 2019-04-19 | 山东源根石油化工有限公司 | A kind of method for purifying and recovering of lubricating oil |
| CN110207017A (en) * | 2019-07-03 | 2019-09-06 | 上海赛科石油化工有限责任公司 | A kind of spent solvent exhaust system and application thereof |
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Application publication date: 20121017 |