CN101768505A - Flocculated-adsorption regeneration treating method for waste engine oil - Google Patents
Flocculated-adsorption regeneration treating method for waste engine oil Download PDFInfo
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Abstract
The invention relates to a flocculated-adsorption regeneration treating method for waste engine oil. The method comprises the following steps of settling filtration, primary flocculation, secondary flocculation, and adsorption bleaching. The impurities, hydrocarbons, carbon deposits, particles, cement gums and the like in the oil can be settled and separated through two flocculation processes, the bleaching property of hydrogen peroxide and the adsorption bleaching property of clay are combined, and then the color, stability and electric property of the oil can be obviously improved. The regeneration method has the advantages of simple process, convenient and safe operation, low investment of regeneration equipment, improvement on the original lubricating oil blending equipment, and suitability for small-scale treatment. The regenerated lubricating oil completely satisfies the applicable national standards. The residue slag generated in the flocculation process can be used as asphalt matching material for paving roads after reprocessing. The good economic benefit can be produced, and the secondary pollution is reduced.
Description
Technical field
The invention belongs to processing exhausted lubricant,, be specifically related to a kind of flocculated-adsorption regeneration treating method for waste engine oil to reclaim useful product technical field.
Background technology
Lubricating oil is the high priced line that is extract by petroleum products, and in the ordinary course of things, if there is 1% hydro carbons rotten in the lubricating oil, this oil just can not continue to have re-used down.Because people lack correct understanding to lubricating oil, the waste oil of replacing often is used as the direct burning of fuel or directly abandons, and has so not only wasted the valuable energy, and has polluted environment.In fact, " waste oil " changed in the normal drain period is useless, and real rotten composition is percentum wherein.As long as impurity in the waste oil and rotten composition are removed, the oil that bears again is to can be used as the base oil of lubricating oil or blend component.Different types of lubricating oil, regenerated technology is not quite similar.In recent years, in the world technology of waste oil regenerating is divided three classes: the first kind is purifying (Reclamation) again, be equivalent to simple regeneration technology, comprise sedimentation, centrifugal, these treatment steps filter, flocculate, but water in the waste oil, general outstanding turbid impurity and with the mechanical impurity of colloidal state stable dispersion are mainly removed in one or several step coupling.Second class is to carry out chemical refining and refining with adsorbents on the basis of back again re-refine (Reprocessing), can regenerate to obtain the lubricating oil, mold oil, clean fuel, the cleaning roads wet goods that use under metal working fluid, the non-severe condition.The 3rd class is re-refine (Refining), be the regenerative process that comprises distillation, as distill a hydrogenation, can produce the regeneration base oil that meets the requirement of natural oil gross, modulate various basic, normal, high shelves oil products, quality is similar to the oil product of producing from natural oil.
Yet along with improving constantly of quality of lubrication oil specification and standard, the kind of additive and consumption are also continuing to increase in the lubricating oil, have increased the difficulty of reclaiming waste lubricating oil technology.Along with the attention of people to environmental protection, the technology that produces secondary pollution in the waste oil regeneration process also will be eliminated gradually simultaneously.In order to satisfy the needs and the environmental requirement of The modern industry development, more advanced lubricating oil regeneration process exploitation is subject to people's attention day by day.
Patent CN101041789A has proposed a kind of waste lubricating oil hydrogenation reproducing method.This method mainly is that waste lubricating oil is implemented dehydration, filtration and adsorption treatment, removes wherein moisture, mechanical impurity, colloid, bituminous matter and most of beavy metal impurity; Then in protectant reactor is housed, carry out pre-hydrofining, further remove impurity; Enter the hydrogenation main reactor at last, realize hydrofining under the effect of hydrogenation catalyst, make the undesirable components hydrogenation in the waste lubricating oil saturated, product carries out the fractionation cutting.
Patent CN1539936 has proposed a kind of solvent extraction and hydrofining bonded waste lubricant oil regeneration method.This method at first adds waste lubricating oil in the alkane solvents, under the condition of 30～130 ℃ of temperature, pressure 3～16MPa, extract, extraction liquid is carried out sedimentation under the condition of 80～150 ℃ of temperature, pressure 3～16MPa, then the extraction liquid after the sedimentation is sent in the alkane solvents recovery tower and separated, in isolated lubricating oil component, feed hydrogen at last, under the effect of hydrogenation catalyst, be that 280～370 ℃, pressure are to carry out hydrofining in the hydrogenator of 3～8MPa in temperature.
Patent CN101033433 has proposed a kind of with distillation and the refining waste lubricant oil regeneration method that combines.Its method is with the waste lubricating oil natural subsidence, removes its water that contains and mechanical impurity, then carries out the normal temperature underpressure distillation, carries out short-path distillation then, at last lubricating oil is carried out carclazyte or solvent treatment and promptly gets the back lubricating oil of regenerating.
But above these waste lubricant oil regeneration treatment technologies need distill or hydrotreatment, and the regenerated reaction conditions requires relatively harsher, and the regenerating unit investment is higher, and the hydrogenation cost only is fit to extensive the processing than costliness.
Summary of the invention
Technical problem to be solved by this invention is to overcome the shortcoming of above-mentioned waste lubricant oil regeneration method, provide that a kind of renovation process is simple, easy and safe to operate, reclaim equiment drop into low, be suitable for the flocculated-adsorption regeneration treating method for waste engine oil handled on a small scale.
Solving the problems of the technologies described above the technical scheme that is adopted is that it is made up of following step:
1, sedimentation is filtered
Get useless engine oil and pack in the container, 65～75 ℃ of sedimentations are 24 hours in thermostat container, get upper strata edible vegetable oil, filter.
2, once flocculation
The adding massfraction is 25% aqueous sodium carbonate in the upper strata edible vegetable oil after step 1 is filtered, massfraction is that the add-on of 25% aqueous sodium carbonate is 1%～6% of a upper strata edible vegetable oil quality, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, change in the thermostat container 70～80 ℃ of sedimentations 16～20 hours over to, naturally cool to room temperature, get the upper strata edible vegetable oil that once flocculates.
3, secondary flocculation
The adding massfraction is polyamide resin-ethanolic soln of 25% in the upper strata edible vegetable oil that once flocculates, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is 2.5%～15% of the upper strata edible vegetable oil quality of once flocculating, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 10 minutes, change in the thermostat container 70～80 ℃ of sedimentations 16～20 hours over to, naturally cool to room temperature, get secondary flocculation upper strata edible vegetable oil.
4, adsorption bleaching
Atlapulgite was put into 120 ℃ of dryings of thermostatic drying chamber 3 hours; Stablizer is joined in the container, add massfraction again and be 30% aqueous hydrogen peroxide solution, the addition of stablizer is that massfraction is 5% of 30% an aqueous hydrogen peroxide solution quality, mixes, and is prepared into the hydrogen peroxide discoloring agent; The secondary upper strata edible vegetable oil that flocculates is heated to 50 ℃, add the hydrogen peroxide discoloring agent, the add-on of hydrogen peroxide discoloring agent is 1%～5% of a secondary flocculation upper strata edible vegetable oil quality, be heated to 60 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, be warming up to 110 ℃, add atlapulgite, be warming up to 150 ℃, add the atlapulgite of equal in quality again, total add-on of atlapulgite is 2%～14% of a secondary flocculation upper strata edible vegetable oil quality, 1000 rev/mins continue to be stirred 30 minutes, changed in the thermostat container 70 ℃ of sedimentations 3 hours over to, got upper strata edible vegetable oil, filter, obtain rerefined oil.
Above-mentioned stablizer is that water glass and sal epsom are the mixture that is hybridly prepared at 7: 1 by mass ratio.
In a flocculation step 2 of the present invention, add massfraction in the upper strata edible vegetable oil after step 1 is filtered and be 25% aqueous sodium carbonate, massfraction is that the preferred add-on of 25% aqueous sodium carbonate is 2%～5% of a upper strata edible vegetable oil quality.In secondary flocculation step 3, add massfraction and be polyamide resin-ethanolic soln of 25% in the upper strata edible vegetable oil that once flocculates, massfraction is that the preferred add-on of polyamide resin-ethanolic soln of 25% is 5%～10% of the upper strata edible vegetable oil quality of once flocculating.In adsorption bleaching step 4, the secondary upper strata edible vegetable oil that flocculates is heated to 50 ℃, add the hydrogen peroxide discoloring agent, the preferred add-on of hydrogen peroxide discoloring agent is 1%～3% of a secondary flocculation upper strata edible vegetable oil quality, is heated to 60 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, be warming up to 110 ℃, add atlapulgite, be warming up to 150 ℃, the atlapulgite that adds equal in quality again, preferred total add-on of atlapulgite are 4%～10% of secondary flocculation upper strata edible vegetable oil quality.
In a flocculation step 2 of the present invention, the adding massfraction is 25% aqueous sodium carbonate in the upper strata edible vegetable oil after step 1 is filtered, massfraction is that the optimal addn of 25% aqueous sodium carbonate is 2% of a upper strata edible vegetable oil quality, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, changed in the thermostat container 70～80 ℃ of best sedimentations 16 hours over to.In secondary flocculation step 3, the adding massfraction is polyamide resin-ethanolic soln of 25% in the upper strata edible vegetable oil that once flocculates, massfraction is that the optimal addn of polyamide resin-ethanolic soln of 25% is 10% of the upper strata edible vegetable oil quality of once flocculating, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 10 minutes, changed in the thermostat container 70～80 ℃ of best sedimentations 16 hours over to.In adsorption bleaching step 4, the secondary upper strata edible vegetable oil that flocculates is heated to 50 ℃, add the hydrogen peroxide discoloring agent, the optimal addn of hydrogen peroxide discoloring agent is 2% of a secondary flocculation upper strata edible vegetable oil quality, is heated to 60 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, be warming up to 110 ℃, add atlapulgite, be warming up to 150 ℃, the atlapulgite that adds equal in quality again, best total add-on of atlapulgite are 10% of secondary flocculation upper strata edible vegetable oil quality.
Flocculated-adsorption regeneration treating method for waste engine oil of the present invention, make well cuts, hydro carbons, carbon deposit, particle, clay etc. settlement separate by twice flocculation process, in conjunction with the bleaching of hydrogen peroxide and the adsorption bleaching of carclazyte, color, stability and the electric property of oil product are obviously improved again.The present invention has the advantage that renovation process is simple, easy and safe to operate, the reclaim equiment input is low, only need be improved, be suitable on the basis of former lubricating oil mediation equipment the small-scale processing, regenerated lubricating oil meets relevant national standard fully, after reprocessing, the waste residue of flocculation process generation simultaneously can be used as the pitch batching of the usefulness of paving the way, can produce favorable economic benefit, reduce secondary pollution.
Embodiment
The present invention is described in more detail below in conjunction with embodiment, but the invention is not restricted to these embodiment.
Embodiment 1
1, sedimentation is filtered
Get the useless engine oil of 1kg and pack in the container, 65～75 ℃ of sedimentations are 24 hours in thermostat container, get upper strata edible vegetable oil, filter.
2, once flocculation
The adding massfraction is 25% aqueous sodium carbonate in the upper strata edible vegetable oil after step 1 is filtered, massfraction is that the add-on of 25% aqueous sodium carbonate is 2% of a upper strata edible vegetable oil quality, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, change in the thermostat container 70～80 ℃ of sedimentations 16 hours over to, naturally cool to room temperature, get the upper strata edible vegetable oil that once flocculates.
3, secondary flocculation
The adding massfraction is polyamide resin-ethanolic soln of 25% in the upper strata edible vegetable oil that once flocculates, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is 10% of the upper strata edible vegetable oil quality of once flocculating, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 10 minutes, change in the thermostat container 70～80 ℃ of sedimentations 16 hours over to, naturally cool to room temperature, get secondary flocculation upper strata edible vegetable oil.
4, adsorption bleaching
Carclazyte was put into 120 ℃ of dryings of thermostatic drying chamber 3 hours; Is to join in container at 7: 1 water glass and sal epsom by mass ratio, as stablizer, add massfraction again and be 30% aqueous hydrogen peroxide solution, the add-on of stablizer is that massfraction is 5% of 30% an aqueous hydrogen peroxide solution quality, mix, be prepared into the hydrogen peroxide discoloring agent; The secondary upper strata edible vegetable oil that flocculates is heated to 50 ℃, add the hydrogen peroxide discoloring agent, the add-on of hydrogen peroxide discoloring agent is 2% of a secondary flocculation upper strata edible vegetable oil quality, be heated to 60 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, be warming up to 110 ℃, add atlapulgite, be warming up to 150 ℃, add the atlapulgite of equal in quality again, total add-on of atlapulgite is 10% of a secondary flocculation upper strata edible vegetable oil quality, 1000 rev/mins continue to be stirred 30 minutes, changed in the thermostat container 70 ℃ of sedimentations 3 hours over to, got upper strata edible vegetable oil, filter, obtain rerefined oil.
Embodiment 2
In a flocculation step 2 of present embodiment, massfraction is that the add-on of 25% aqueous sodium carbonate is 1% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.In secondary flocculation step 3, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is 2.5% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.In adsorption bleaching step 4, the add-on of hydrogen peroxide discoloring agent is 1% of a secondary flocculation upper strata edible vegetable oil quality, and total add-on of atlapulgite is 2% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, obtain rerefined oil.
Embodiment 3
In a flocculation step 2 of present embodiment, massfraction is that the add-on of 25% aqueous sodium carbonate is 6% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.Coagulate in the step 3 at secondary, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is 15% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.In adsorption bleaching step 4, the add-on of hydrogen peroxide discoloring agent is 5% of a secondary flocculation upper strata edible vegetable oil quality, and total add-on of atlapulgite is 14% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, obtain rerefined oil.
Embodiment 4
In a flocculation step 2 of present embodiment, massfraction is that the add-on of 25% aqueous sodium carbonate is 5% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.In secondary flocculation step 3, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is 5% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.In adsorption bleaching step 4, the add-on of hydrogen peroxide discoloring agent is 3% of a secondary flocculation upper strata edible vegetable oil quality, and total add-on of atlapulgite is 4% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, obtain rerefined oil.
Embodiment 5
In a flocculation step 2 of present embodiment, massfraction is that the add-on of 25% aqueous sodium carbonate is 4% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.In secondary flocculation step 3, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is 7.5% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.In adsorption bleaching step 4, the add-on of hydrogen peroxide discoloring agent is 4% of a secondary flocculation upper strata edible vegetable oil quality, and total add-on of atlapulgite is 8% of a upper strata edible vegetable oil quality, and other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, obtain rerefined oil.
Embodiment 6
In a flocculation step 2 of the foregoing description 1～5, change in the thermostat container 70～80 ℃ of sedimentations 20 hours over to, other steps of this step are identical with respective embodiments.In secondary flocculation step 3, change in the thermostat container 70～80 ℃ of sedimentations 20 hours over to, other steps of this step are identical with respective embodiments.Other steps are identical with respective embodiments, obtain rerefined oil.
Embodiment 7
In a flocculation step 2 of the foregoing description 1～5, change in the thermostat container 70～80 ℃ of sedimentations 18 hours over to, other steps of this step are identical with respective embodiments.In secondary flocculation step 3, change in the thermostat container 70～80 ℃ of sedimentations 18 hours over to, other steps of this step are identical with respective embodiments.Other steps are identical with respective embodiments, obtain rerefined oil.
In order to determine optimum process condition of the present invention, the contriver has carried out a large amount of laboratory study tests, and various test situation are as follows:
Testing method: GB/T 511 " petroleum products and additive mechanical impurity assay method (weighting method) " measures mechanical impurity; GB/T 264 " petroleum products determination of acid value method " measures acid number; GB/T 508 " petroleum products determination of ash method " measures ash content; SH/T 0168 " chromaticity of petroleum product assay method " measures colourity.
1, aqueous sodium carbonate concentration is to the influence of quality of reclaimed
Get useless engine oil 10kg, 75 ℃ of sedimentations are 24 hours in thermostat container, get upper strata edible vegetable oil, filter, get totally 6 parts of upper strata edible vegetable oil 1kg after the filtration, place container respectively, add the 0.02kg massfraction respectively and be 5%, 10%, 15%, 20%, 25%, 30% aqueous sodium carbonate, the add-on of aqueous sodium carbonate all is 2% of upper strata edible vegetable oil quality, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, changed in the thermostat container 75 ℃ of sedimentations 16 hours over to, naturally cool to room temperature, get the upper strata edible vegetable oil that once flocculates.Other steps are identical with embodiment 1.Obtain rerefined oil.Test result sees Table 1.
Table 1 aqueous sodium carbonate concentration is to the influence of quality of reclaimed
| Concentration (%) | ??5 | ??10 | ??15 | ??20 | ??25 | ??30 |
| Mechanical impurity (%) | ??0.0010 | ??0.0009 | ??0.0008 | ??0.0006 | ??0.0004 | ??0.0009 |
| Acid number (mgKOH/g) | ??0.25 | ??0.21 | ??0.18 | ??0.15 | ??0.08 | ??0.12 |
| Ash content (%) | ??0.18 | ??0.15 | ??0.13 | ??0.11 | ??0.05 | ??0.10 |
| Colourity (number) | Less than 5.5 | Less than 4.5 | Less than 4 | Less than 3.5 | Less than 3 | Less than 3 |
By table 1 as seen, the massfraction of aqueous sodium carbonate is 25% o'clock, and the mechanical impurity of the rerefined oil that obtains, acid number, ash content, colourity all reach lower level.It is 25% aqueous sodium carbonate that the present invention selects massfraction.
2, the aqueous sodium carbonate add-on is to the influence of quality of reclaimed
Get useless engine oil 10kg, 75 ℃ of sedimentations are 24 hours in thermostat container, get upper strata edible vegetable oil, filter, get totally 6 parts of upper strata edible vegetable oil 1kg after the filtration, place container respectively, add 0.01kg respectively, 0.02kg, 0.03kg, 0.04kg, 0.05kg, 0.06kg massfraction is 25% aqueous sodium carbonate, massfraction is that the add-on of 25% aqueous sodium carbonate is respectively 1% of a upper strata edible vegetable oil quality, 2%, 3%, 4%, 5%, 6%, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, changed in the thermostat container 75 ℃ of sedimentations 16 hours over to, naturally cool to room temperature, get the upper strata edible vegetable oil that once flocculates.Other steps are identical with embodiment 1.Obtain rerefined oil.Test result sees Table 2.
Table 2 aqueous sodium carbonate add-on is to the influence of quality of reclaimed
| Concentration (%) | ??1 | ??2 | ??3 | ??4 | ??5 | ??6 |
| Mechanical impurity (%) | ??0.0009 | ??0.0004 | ??0.0004 | ??0.0006 | ??0.0005 | ??0.0004 |
| Acid number (mgKOH/g) | ??0.18 | ??0.08 | ??0.11 | ??0.12 | ??0.12 | ??0.15 |
| Ash content (%) | ??0.18 | ??0.05 | ??0.10 | ??0.11 | ??0.12 | ??0.13 |
| Concentration (%) | ??1 | ??2 | ??3 | ??4 | ??5 | ??6 |
| Colourity (number) | Less than 4.5 | Less than 3 | Less than 3.5 | Less than 4 | Less than 4 | Less than 4 |
By table 2 as seen, massfraction is that 25% aqueous sodium carbonate add-on is 1%～6% o'clock of upper strata edible vegetable oil quality, and the mechanical impurity of the rerefined oil that obtains, acid number, ash content, colourity all reach lower level.The present invention select massfraction be the add-on of 25% aqueous sodium carbonate be sedimentation filter upper strata, back edible vegetable oil quality 1%～6%, the best is 2%.
3, polyamide resin-ethanolic soln concentration is to the influence of quality of reclaimed
Get useless engine oil 10kg, method according to embodiment 1, filter through sedimentation, once flocculation, upper strata edible vegetable oil is once flocculated, get totally 6 parts of the upper strata edible vegetable oil 1kg of once flocculating, place container respectively, adding the 0.10kg massfraction respectively is 10%, 15%, 20%, 25%, 30%, polyamide resin-ethanolic soln of 35%, the add-on of polyamide resin-ethanolic soln all is 10% of the upper strata edible vegetable oil quality of once flocculating, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 10 minutes, changed in the thermostat container 75 ℃ of sedimentations 16 hours over to, naturally cool to room temperature, get secondary flocculation upper strata edible vegetable oil.Other steps are identical with embodiment 1.Obtain rerefined oil.Test result sees Table 3.
Table 3 polyamide resin-ethanolic soln concentration is to the influence of quality of reclaimed
| Concentration (%) | ??10 | ??15 | ??20 | ??25 | ??30 | ??35 |
| Mechanical impurity (%) | ??0.0005 | ??0.0006 | ??0.0005 | ??0.0004 | ??0.0014 | ??0.0015 |
| Acid number (mgKOH/g) | ??0.13 | ??0.010 | ??0.09 | ??0.08 | ??0.09 | ??0.08 |
| Ash content (%) | ??0.17 | ??0.15 | ??0.12 | ??0.05 | ??0.05 | ??0.06 |
| Colourity (number) | Less than 4.5 | Less than 4 | Less than 3 | Less than 3 | Less than 3 | Less than 3 |
By table 3 as seen, polyamide resin-ethanolic soln massfraction is 25% o'clock, and the mechanical impurity of the rerefined oil that obtains, acid number, ash content, colourity all reach lower level.It is polyamide resin-ethanolic soln of 25% that the present invention selects massfraction.
4, polyamide resin-ethanolic soln add-on is to the influence of quality of reclaimed
Get useless engine oil 10kg, method according to embodiment 1, filter through sedimentation, once flocculation, upper strata edible vegetable oil is once flocculated, get totally 6 parts of the upper strata edible vegetable oil 1kg of once flocculating, place container respectively, add 0.025kg respectively, 0.050kg, 0.075kg, 0.100kg, 0.125kg, 0.150kg massfraction is polyamide resin-ethanolic soln of 25%, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is respectively 2.5% of the upper strata edible vegetable oil quality of once flocculating, 5%, 7.5%, 10%, 12.5%, 15%, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 10 minutes, change in the thermostat container 75 ℃ of sedimentations 16 hours over to, naturally cool to room temperature, get secondary flocculation upper strata edible vegetable oil.Other steps are identical with embodiment 1.Obtain rerefined oil.Test result sees Table 4.
Table 4 polyamide resin-ethanolic soln add-on is to the influence of quality of reclaimed
| Concentration (%) | ??2.5 | ??5 | ??7.5 | ??10 | ??12.5 | ??15 |
| Mechanical impurity (%) | ??0.0008 | ??0.0005 | ??0.0006 | ??0.0004 | ??0.0005 | ??0.0005 |
| Acid number (mgKOH/g) | ??0.13 | ??0.12 | ??0.10 | ??0.08 | ??0.12 | ??0.13 |
| Ash content (%) | ??0.19 | ??0.15 | ??0.11 | ??0.05 | ??0.13 | ??0.12 |
| Colourity (number) | Less than 4.5 | Less than 3.5 | Less than 3 | Less than 3 | Less than 3 | Less than 3 |
By table 4 as seen, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is 2.5%～15% o'clock of the upper strata edible vegetable oil quality of once flocculating, and the mechanical impurity of the rerefined oil that obtains, acid number, ash content, colourity all reach lower level.It is that the add-on of polyamide resin-ethanolic soln of 25% is 2.5%～15% of the upper strata edible vegetable oil quality of once flocculating that the present invention selects massfraction, and the best is 10%.
5, hydrogen peroxide discoloring agent add-on is to the influence of decolorizing effect
Get useless engine oil 10kg, method according to embodiment 1, filter through sedimentation, once flocculation, the secondary flocculation, obtain secondary flocculation upper strata edible vegetable oil, get totally 6 parts of secondary flocculation upper strata edible vegetable oil 1kg, place container respectively, be heated to 50 ℃, 1000 rev/mins of stirrings, add hydrogen peroxide discoloring agent 0kg respectively, 0.01kg, 0.02kg, 0.03kg, 0.04kg, 0.05kg, the add-on of hydrogen peroxide discoloring agent is respectively 0% of a secondary flocculation upper strata edible vegetable oil quality, 1%, 2%, 3%, 4%, 5%, be heated to 60 ℃, 1000 rev/mins of constant temperature stirred 20 minutes.Other steps are identical with embodiment 1.Obtain rerefined oil.
Test result sees Table 5.
Table 5 hydrogen peroxide discoloring agent add-on is to the influence of decolorizing effect
| Add-on (%) | ??0 | ??1 | ??2 | ??3 | ??4 | ??5 |
| Mechanical impurity (%) | ??0.0005 | ??0.0004 | ??0.0004 | ??0.0005 | ??0.0004 | ??0.0006 |
| Acid number (mgKOH/g) | ??0.12 | ??0.11 | ??0.08 | ??0.10 | ??0.11 | ??0.11 |
| Ash content (%) | ??0.11 | ??0.10 | ??0.05 | ??0.11 | ??0.11 | ??0.10 |
| Colourity (number) | Less than 5.5 | Less than 4.0 | Less than 3 | Less than 3.5 | Less than 3.5 | Less than 3.5 |
By table 5 as seen, the mechanical impurity of the rerefined oil that obtains, acid number, ash content all reach lower level, and colourity afterwards rises with first decline of the increase of hydrogen peroxide discoloring agent add-on, and add-on is 2% o'clock of secondary flocculation upper strata edible vegetable oil quality, the colourity minimum.It is 1%～5% of secondary flocculation upper strata edible vegetable oil quality that the present invention selects the add-on of hydrogen peroxide discoloring agent, and the best is 2%.
6, the atlapulgite add-on is to the influence of decolorizing effect
Get useless engine oil 10kg, method according to embodiment 1, filter through sedimentation, once flocculation, the secondary flocculation, obtain secondary flocculation upper strata edible vegetable oil, get totally 7 parts of secondary flocculation upper strata edible vegetable oil 1kg, place container respectively, be heated to 50 ℃, 1000 rev/mins of stirrings add 0.02kg hydrogen peroxide discoloring agent, the add-on of hydrogen peroxide discoloring agent be secondary flocculation upper strata edible vegetable oil quality 2%, be heated to 60 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, were warming up to 110 ℃, added 0kg respectively, 0.01kg, 0.02kg, 0.04kg, 0.05kg, 0.06kg, 0.07kg atlapulgite, be warming up to 150 ℃, the atlapulgite that adds equal in quality again, total add-on of atlapulgite are respectively 0% of secondary flocculation upper strata edible vegetable oil quality, 2%, 4%, 8%, 10%, 12%, 14%, 1000 rev/min is continued to stir 30 minutes, change in the thermostat container 70 ℃ of sedimentations 3 hours over to, get upper strata edible vegetable oil, filter, obtain rerefined oil.Test result sees Table 6.
Table 6 atlapulgite add-on is to the influence of decolorizing effect
| Add-on (%) | ??0 | ??2 | ??4 | ??8 | ??10 | ??12 | ??14 |
| Mechanical impurity (%) | ??0.0004 | ??0.0005 | ??0.0003 | ??0.0006 | ??0.0004 | ??0.0005 | ??0.0004 |
| Acid number (mgKOH/g) | ??0.12 | ??0.10 | ??0.12 | ??0.11 | ??0.08 | ??0.12 | ??0.11 |
| Ash content (%) | ??0.11 | ??0.10 | ??0.11 | ??0.10 | ??0.05 | ??0.11 | ??0.10 |
| Colourity (number) | Less than 7.5 | Less than 4.5 | Less than 4 | Less than 3.5 | Less than 3 | Less than 3 | Less than 3 |
The mechanical impurity of the rerefined oil that by table 6 as seen, obtains, acid number, ash content, colourity all reach lower level.The total add-on of atlapulgite is 2%～14% o'clock of secondary flocculation upper strata edible vegetable oil quality, and decolorizing effect is better, and wherein add-on is 10% o'clock, and decolorizing effect is best, continues to increase the add-on of atlapulgite, and decolorizing effect is constant substantially.It is 2%～14% of secondary flocculation upper strata edible vegetable oil quality that the present invention selects total add-on of atlapulgite, and the best is 10%.
In order to determine beneficial effect of the present invention, the contriver tests to commercially available engine oil (model is SF 10W/30), useless engine oil and according to the embodiment of the invention 1 flocculated-adsorption regeneration treating method for waste engine oil rerefined oil that obtains after the engine oil manipulation of regeneration that will give up, and various test case are as follows:
Laboratory apparatus: petroleum densitmeter, produce by Shanghai Medical Instrument and Meter Factory; SYD-265C petroleum products kinematic viscosity tester is produced by Shanghai Changji Geological Instrument Co., Ltd.; SYD-3536 Cleveland open cup flash test device is produced by Shanghai Changji Geological Instrument Co., Ltd.; SYD-30011 numerical control electric furnace process coke test device is produced by Shanghai Changji Geological Instrument Co., Ltd.; Box resistance box is produced by Shanghai City laboratory apparatus head factory; The chromaticity of petroleum product determinator is produced by Shanghai Peng Pu refrigerator head factory; The accurate reinforcement electric mixer of JJ-1 is produced by Shanghai Pudong Physical and Optical Instruments Factory.
Testing method: measure 20 ℃ of density according to GB/T 1884 " crude oil and liquid petroleum product density experiment chamber assay method (densimeter method) "; GB/T265 " petroleum products kinematic viscosity assay method " measures 40 ℃, 100 ℃ kinematic viscosities; GB/T 3536 " petroleum products flash-point and determination of ignition point method (Cleveland opening agar diffusion method) " measures open flash point; GB/T511 " petroleum products and additive mechanical impurity assay method (weighting method) " measures mechanical impurity; SH/T 0170 " petroleum products Conradson method (electric furnace process) " measures the carbon residue amount; GB/T 508 " petroleum products determination of ash method " measures ash content; GB/T 264 " petroleum products determination of acid value method " measures acid number; SH/T 0168 " chromaticity of petroleum product assay method " measures colourity; GB/T 3535 " petroleum sneeze-point assay method " measures pour point.Detected result sees Table 7.
Table 7 physical and chemical index simultaneous test detected result
By table 7 as seen, the physical and chemical index of every physical and chemical index of employing the inventive method regenerated lubricating oil and commercially available SF 10W/30 h type engine h lubricating oil is approaching.
Claims (3)
1. flocculated-adsorption regeneration treating method for waste engine oil is characterized in that it is made up of following step:
(1) sedimentation is filtered
Get useless engine oil and pack in the container, 65～75 ℃ of sedimentations are 24 hours in thermostat container, get upper strata edible vegetable oil, filter;
(2) once flocculation
The adding massfraction is 25% aqueous sodium carbonate in the upper strata edible vegetable oil after step 1 is filtered, massfraction is that the add-on of 25% aqueous sodium carbonate is 1%～6% of a upper strata edible vegetable oil quality, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, change in the thermostat container 70～80 ℃ of sedimentations 16～20 hours over to, naturally cool to room temperature, get the upper strata edible vegetable oil that once flocculates;
(3) secondary flocculation
The adding massfraction is polyamide resin-ethanolic soln of 25% in the upper strata edible vegetable oil that once flocculates, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is 2.5%～15% of the upper strata edible vegetable oil quality of once flocculating, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 10 minutes, change in the thermostat container 70～80 ℃ of sedimentations 16～20 hours over to, naturally cool to room temperature, get secondary flocculation upper strata edible vegetable oil;
(4) adsorption bleaching
Atlapulgite was put into 120 ℃ of dryings of thermostatic drying chamber 3 hours; Stablizer is joined in the container, add massfraction again and be 30% aqueous hydrogen peroxide solution, the addition of stablizer is that massfraction is 5% of 30% an aqueous hydrogen peroxide solution quality, mixes, and is prepared into the hydrogen peroxide discoloring agent; The secondary upper strata edible vegetable oil that flocculates is heated to 50 ℃, add the hydrogen peroxide discoloring agent, the add-on of hydrogen peroxide discoloring agent is 1%～5% of a secondary flocculation upper strata edible vegetable oil quality, be heated to 60 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, be warming up to 110 ℃, add atlapulgite, be warming up to 150 ℃, add the atlapulgite of equal in quality again, total add-on of atlapulgite is 2%～14% of a secondary flocculation upper strata edible vegetable oil quality, 1000 rev/mins continue to be stirred 30 minutes, changed in the thermostat container 70 ℃ of sedimentations 3 hours over to, got upper strata edible vegetable oil, filter, obtain rerefined oil;
Above-mentioned stablizer is that water glass and sal epsom are the mixture that is hybridly prepared at 7: 1 by mass ratio.
2. according to the described flocculated-adsorption regeneration treating method for waste engine oil of claim 1, it is characterized in that: in a flocculation step (2), add massfraction in the upper strata edible vegetable oil after step (1) is filtered and be 25% aqueous sodium carbonate, massfraction is that the add-on of 25% aqueous sodium carbonate is 2%～5% of a upper strata edible vegetable oil quality; In secondary flocculation step (3), in the upper strata edible vegetable oil that once flocculates, add massfraction and be polyamide resin-ethanolic soln of 25%, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is 5%～10% of the upper strata edible vegetable oil quality of once flocculating; In adsorption bleaching step (4), the secondary upper strata edible vegetable oil that flocculates is heated to 50 ℃, add the hydrogen peroxide discoloring agent, the add-on of hydrogen peroxide discoloring agent is 1%～3% of a secondary flocculation upper strata edible vegetable oil quality, is heated to 60 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, be warming up to 110 ℃, add atlapulgite, be warming up to 150 ℃, the atlapulgite that adds equal in quality again, total add-on of atlapulgite are 4%～10% of secondary flocculation upper strata edible vegetable oil quality.
3. according to the described flocculated-adsorption regeneration treating method for waste engine oil of claim 1, it is characterized in that: in a flocculation step (2), the adding massfraction is 25% aqueous sodium carbonate in the upper strata edible vegetable oil after step 1 is filtered, massfraction is that the add-on of 25% aqueous sodium carbonate is 2% of a upper strata edible vegetable oil quality, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, changed in the thermostat container 70～80 ℃ of sedimentations 16 hours over to; In secondary flocculation step (3), the adding massfraction is polyamide resin-ethanolic soln of 25% in the upper strata edible vegetable oil that once flocculates, massfraction is that the add-on of polyamide resin-ethanolic soln of 25% is 10% of the upper strata edible vegetable oil quality of once flocculating, be heated to 75 ℃, 1000 rev/mins of constant temperature stirred 10 minutes, changed in the thermostat container 70～80 ℃ of sedimentations 16 hours over to; In adsorption bleaching step (4), the secondary upper strata edible vegetable oil that flocculates is heated to 50 ℃, add the hydrogen peroxide discoloring agent, the add-on of hydrogen peroxide discoloring agent is 2% of a secondary flocculation upper strata edible vegetable oil quality, is heated to 60 ℃, 1000 rev/mins of constant temperature stirred 20 minutes, be warming up to 110 ℃, add atlapulgite, be warming up to 150 ℃, the atlapulgite that adds equal in quality again, total add-on of atlapulgite are 10% of secondary flocculation upper strata edible vegetable oil quality.
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| CN102167993A (en) * | 2010-11-25 | 2011-08-31 | 豆远奎 | Method for purifying waste engine oil containing phosphating film |
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