Waste lubricant oil by hydrogenation process for purification and hydrofinishing system
Technical field
The invention belongs to technical field of lubricating oil, and in particular to a kind of waste lubricant oil by hydrogenation process for purification and hydrofinishing system
System.
Background technology
Lubricating oil is extract in oil with high value-added product, usually by lube base oil and lubricating oil
The compositions such as additive.Lubricating oil can cause in use because of physics, chemistry or the factors such as artificial its property occur fission or
Impurity etc. is mixed into, its quality is made to be lower and becomes waste lubricating oil.By suitable technical matters by waste lubricant oil regeneration, change into
The reclaimed oil that can be re-used, no matter from the perspective of technology, environmental protection, the utilization of resources and economy, all with important
Realistic meaning.
Traditional process for regeneration of waste lubricating oil is mainly sulfuric acid-carclazyte method, including purification, pickling, clay-filtered and fractionation
Step, purifying step include sedimentation, filtering, coalescence, vacuum flashing, mainly remove water, part light oil and mechanical admixture.It should
The shortcomings that technique productions is that quality of reclaimed is poor, and the rate of recovery is low, and secondary pollution is serious.With quality of lubrication oil specification and standard
Continuous improvement, the species of additive and dosage are also continuing to increase in lubricating oil, add reclaiming waste lubricating oil technique
Difficulty;Simultaneously with the attention of people's environmental protection, the technology of generation secondary pollution also will gradually be eliminated in waste oil regeneration technology.
These situations all promote the appearance of more advanced process for regeneration of waste lubricating oil.
Waste lubricant oil by hydrogenation process for refining is subject to more next because it has the higher feature of environmental protection, economy and operability
More concerns can significantly improve the quality and quality of product by Hydrofining Technology.However, at the hydrogenation reported at present
The method of reason waste lubricating oil still has several drawbacks part:(1) undesirable components that cannot be sufficiently separated in waste lubricating oil, especially
It is that cannot effectively remove the impurity such as heavy metal element, pitch, colloid;(2) utilization rate of waste lubricating oil raw material is low, and raw material is relied on
Strong, the bad adaptability of property;(3) after hydrotreating, lubricating oil property makes moderate progress, but colourity is big, and light stability and thermostability are poor,
Product easily changes colour and precipitates, and product quality is not high;(4) low yield fails to solve potentially to pollute, and fails fundamentally to solve
The problem of certainly waste lubricant oil regeneration comprehensively utilizes, market adaptability shortcoming.
In consideration of it, special propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of waste lubricant oil by hydrogenation process for purification, simple for process, and operation is flexible, ring
Border is friendly, can effectively remove the de- of the undesirable components in waste lubricating oil, the especially impurity such as heavy metal, colloid, asphalitine
Except significant effect, the yield of Reclaimed Base Oil is improved while Reclaimed Base Oil quality is improved.
The second object of the present invention is to provide a kind of waste lubricant oil by hydrogenation refining system, can be realized pair by the system
The abundant regeneration of waste lubricating oil, the service cycle of device is long, and the service life of catalyst is long, is improving product quality and yield
Advantageously reduce production cost simultaneously.
To achieve the above object, the technical solution adopted by the present invention is:
According to an aspect of the present invention, the present invention provides a kind of waste lubricant oil by hydrogenation process for purification, comprises the following steps:
(a) waste oil pre-processes:Waste lubricating oil is dehydrated and is cleaned pretreatment;
(b) flash:Pretreated waste lubricating oil is flashed, removes traces of moisture and light component;
(c) propane extracts:Waste lubricating oil after flash distillation enters propane extraction tower, is extracted using propane as extractant,
Materials at bottom of tower after the completion of extraction enters pitch propane recovery tower, recycles propane, and tower top material enters supercritical propane recovery tower,
Obtain intermediate product;
(d) distill:Distillation processing is carried out to the intermediate product, to slough heavy constituent in the intermediate product and residual
Charcoal obtains hydrogenation distillate;
(e) hydrofinishing:The hydrogenation distillate is after decompression into the hydrogenation being composed in series by least three reactors
Hydrofinishing is carried out in device, obtains hydrogenated base oil;
(f) it is evaporated under reduced pressure:Hydrogenated base oil is evaporated under reduced pressure, and carries out fraction cutting, obtains different grades of add
Hydrogen regenerates oil product.
As further preferred technical solution, the pretreatment of waste oil in step (a) include the filtering carried out successively, demulsification and
Backwash filter.
As further preferred technical solution, in the filtration step, the strainer mesh number used is 60~100 mesh, preferably
For 70~90 mesh, further preferably 80 mesh;
Preferably, the demulsification step includes:The waste lubricating oil obtained after filtering is heated to 80~150 DEG C, is added in de-
Brine and demulsifier carry out washing demulsification, after settling 5~8h, discharge bottom moisture and mechanical admixture;
Preferably, the backwash filter step includes:The waste lubricating oil obtained after sedimentation enters automatic back flush filtration
In device, backwash filter is carried out in the case where temperature is 50~130 DEG C;
Preferably, multiple strainers are equipped in automatic backwashing filter, the filtering accuracy of strainer is 20~100 μm, preferably
For 25~80 μm.
As further preferred technical solution, the flash temperature in step (b) is 100~260 DEG C, and vacuum degree is -0.01
~-0.09Mpa.
As further preferred technical solution, the propane extraction conditions in step (c) includes:The body of waste lubricating oil and propane
Product is than being 1:2~6, extraction temperature is 50~120 DEG C, and extracting pressure is 3.5~4.3Mpa;
Preferably, the operating condition of supercritical propane recovery tower includes:Operating temperature is 100~150 DEG C, pressure 3.9
~4.5Mpa.
As further preferred technical solution, step (d) includes:
(d1) intermediate product enters vacuum distillation tower, and operating temperature is 300~390 DEG C, and vacuum degree is -0.05
Waste lubricating oil is divided into multiple components by~-0.098Mpa according to boiling range and viscosity;
(d2) intermediate product steams tower into thick, and operating temperature is 350~400 DEG C, vacuum degree for -0.01~-
0.099Mpa sloughs heavy constituent and carbon residue, obtains hydrogenation distillate.
As further preferred technical solution, the hydrogenation plant in step (e) includes three reactors being in series, successively
Include Ni-Co-Mo/Al for the first reactor of filling protective agent and metal remover, filling2O3The second of hydrogenation catalyst is anti-
It answers device and loads the 3rd reactor of antichlor;
Preferably, the condition of hydrofinishing includes:Extraction temperature be 300~365 DEG C, pressure be 4~15Mpa, hydrogen oil body
For product than being 80~1500, liquid volume air speed is 0.1~1.5h- 1。
As further preferred technical solution, step (e) includes hydrofinishing and post-refining, and device used includes phase
The hydrogenation plant and supplementary device of series connection, the hydrogenation plant include three reactors being in series, are followed successively by filling protective agent
First reactor, filling with metal remover include Ni-Co-Mo/Al2O3The second reactor of hydrogenation catalyst and filling
3rd reactor of antichlor, the supplementary device are to be in series and loaded including Ni-Co-Mo- with the 3rd reactor
Pd/Al2O34th reactor of aromatic hydrocarbon refining agent;
Preferably, the condition of hydrofinishing includes:Extraction temperature be 300~365 DEG C, pressure be 4~15Mpa, hydrogen oil body
For product than being 80~1500, liquid volume air speed is 0.1~1.5h- 1;
Preferably, the condition of post-refining includes:Extraction temperature be 275~300 DEG C, pressure be 4~15Mpa, hydrogen oil body
For product than being 80~1500, liquid volume air speed is 0.1~1.5h- 1。
As further preferred technical solution, the step of stripping is further included between step (f) and step (e), hydrogenation basis
Oil is into stripper, and under the conditions of temperature is 200~300 DEG C, the hydrogen sulfide and ammonia of removal hydrogenation reaction generation are stripped
Product;
Preferably, step (f) includes:
(f1) stripped product enters decompression separation tower, and operating temperature is 100~300 DEG C, vacuum degree for -0.05~-
0.098Mpa removes light component caused by hydrocracking;
(f2) stripped product enters vacuum distillation tower, and operating temperature is 300~370 DEG C, vacuum degree for -0.05~-
0.098Mpa carries out fraction cutting according to boiling range and viscosity, obtains different grades of hydrogenation regeneration oil product.
According to another aspect of the present invention, the present invention provides a kind of waste lubricant oil by hydrogenation refining system, includes successively:
Pretreatment unit, to remove the moisture and mechanical admixture in waste lubricating oil;
Flash tank, to remove remaining traces of moisture and light component in waste lubricating oil;
Propane extraction tower, pitch propane recovery tower and supercritical propane recovery tower, with remove the additive in waste lubricating oil,
Colloid, asphalitine and heavy metal, recycling propane and acquisition intermediate product;
Destilling tower, to remove the heavy constituent and carbon residue in intermediate product;
Hydrogenation plant to increase the saturated hydrocarbon content of lubricating oil and remove remaining impurity, obtains hydrogenated base oil;
And vacuum distillation tower, to isolate the base oil fractions in hydrogenated base oil, obtain hydrogenation regeneration oil product.
Compared with prior art, the beneficial effects of the present invention are:
1st, waste lubricant oil by hydrogenation process for purification of the invention, by pre-processing, flashing, propane extracts, distillation, hydrofinishing
With the combination of the techniques such as vacuum distillation, no-float between various techniques obtains comprehensive trade-off effect, realizes to useless
The abundant regeneration of lubricating oil also improves the yield of Reclaimed Base Oil while Reclaimed Base Oil quality is greatly improved.
The present invention is provided with propane extraction and distillation technique before hydrofinishing, and waste lubricating oil removes pitch by propane
After matter and colloid, the impurity such as more than 90% additive and heavy metal in waste lubricating oil can be removed, are realized to weight in waste lubricating oil
The abundant removing of the impurity such as metal, colloid, asphalitine, additive avoids above-mentioned impurity to the equipment during subsequently distilling etc.
The phenomenon that coking etc. is caused to damage equipment, prevents system jams, extends the equipment cycle of operation, ensure the even running of device,
Improve the rate of recovery and quality simultaneously.
2nd, hydrofinishing process of the invention, Reclaimed Base Oil high income, general yield can reach more than 85%.
3rd, good by the obtained Reclaimed Base Oil quality of method of the present invention, viscosity index (VI) can be improved to more than 110, metal
Total amount can be reduced to more than 50ppm, while improve the properties such as acid value, color, photostability and oxidation stability.
4th, hydrofinishing process of the invention, flow is simple, and operation is flexible, and condition mitigates, and will not generate spent acid in the process
The wastes such as slag, spent bleaching clay avoid the introducing of secondary pollution, environmental-friendly;Good product quality after regeneration, high income, equipment
Service life is long, and operating cost is low, balances the relation of environmental protection, resource regeneration and financial cost well.
5th, waste lubricant oil by hydrogenation refining system of the invention, by the system can realize to waste lubricating oil fully again
It is raw, oil quality is improved, and the service cycle of device is long, and equipment investment is few, and the service life of catalyst is long, is improving product
Production cost is advantageously reduced while quality and yield, there is great commercial introduction value.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution of the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in describing below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, can also be obtained according to these attached drawings other attached drawings.
Fig. 1 is waste lubricant oil by hydrogenation refining system structure diagram provided in an embodiment of the present invention.
Icon:1- pretreatment units;2- flash tanks;3- propane extraction towers;4- supercritical propane recovery towers;5- is dripped
Blue or green propane recovery tower;6- destilling towers;7- first reactors;8- second reactors;The 3rd reactors of 9-;10- the 4th reacts
Device;11- strippers;12- vacuum towers.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment and embodiment, but this field skill
Art personnel will be understood that following embodiments and embodiment are merely to illustrate the present invention, and be not construed as the model of the limitation present invention
It encloses.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work
Every other embodiment, belongs to the scope of protection of the invention.
In a first aspect, providing a kind of waste lubricant oil by hydrogenation process for purification in some embodiments, comprise the following steps:
(a) waste oil pre-processes:Waste lubricating oil is dehydrated and is cleaned pretreatment;
(b) flash:Pretreated waste lubricating oil is flashed, removes traces of moisture and light component;
(c) propane extracts:Waste lubricating oil after flash distillation enters propane extraction tower, is extracted using propane as extractant,
Materials at bottom of tower after the completion of extraction enters pitch propane recovery tower, recycles propane, and tower top material enters supercritical propane recovery tower,
Obtain intermediate product;
(d) distill:Distillation processing is carried out to the intermediate product, to slough heavy constituent in the intermediate product and residual
Charcoal obtains hydrogenation distillate;
(e) hydrofinishing:The hydrogenation distillate is after decompression into the hydrogenation being composed in series by least three reactors
Hydrofinishing is carried out in device, obtains hydrogenated base oil;
(f) it is evaporated under reduced pressure:Hydrogenated base oil is evaporated under reduced pressure, and carries out fraction cutting, obtains different grades of add
Hydrogen regenerates oil product.
The present invention first pre-processes waste lubricating oil, eliminates some moisture, mechanical admixture and granule foreign etc.;So
After distilled to remove remaining traces of moisture and light component in waste lubricating oil;Waste lubricating oil after flash distillation enters propane extraction
Tower is extracted using propane as extractant, can remove additive, colloid, asphalitine and heavy metal in waste lubricating oil, extraction
Materials at bottom of tower after the completion of taking enters pitch propane recovery tower, recycles propane, and tower top material enters supercritical propane recovery tower, returns
It receives propane and obtains intermediate product simultaneously, the propane after recycling can be again introduced into propane extraction tower to reuse;Then will obtain
Intermediate product carry out distillation processing, to remove the impurity such as heavy constituent and carbon residue in intermediate product, obtain hydrogenation distillate;So
Obtained hydrogenation distillate is subjected to hydrofinishing afterwards, to increase the saturated hydrocarbon content of lubricating oil and remove remaining impurity, is obtained
Hydrogenated base oil;Finally obtained hydrogenated base oil is evaporated under reduced pressure, and fraction is carried out according to different fractions and viscosity and is cut
It cuts, obtains different grades of hydrogenation regeneration oil product.
In this way, by pre-processing, flashing, propane extract, distillation, organic knot of the techniques such as hydrofinishing and vacuum distillation
It closes, no-float between various techniques obtains comprehensive trade-off effect, the abundant regeneration to waste lubricating oil realized, very big
The yield of Reclaimed Base Oil is also improved while improving Reclaimed Base Oil quality;The yield of Reclaimed Base Oil generally can reach
More than 85%;Viscosity index (VI) can be improved to more than 110, and total metal content can be reduced to more than 50ppm, while improve acid value, face
The properties such as color, photostability and oxidation stability.
Especially prominent, the present invention is provided with propane extraction and distillation technique, waste lubricating oil warp before hydrofinishing
After crossing propane removing asphalitine and colloid, the impurity such as more than 90% additive and heavy metal in waste lubricating oil can be removed, are realized
Abundant removing to the impurity such as heavy metal, colloid, asphalitine, additive in waste lubricating oil avoids above-mentioned impurity to subsequently distilling
The phenomenon that equipment Deng during causes coking etc. to damage equipment, prevents system jams, extends the equipment cycle of operation, ensures dress
The even running put, while improve the rate of recovery and quality.
Above method flow is simple, and operation is flexible, and condition mitigates, and environmental-friendly, low energy consumption, and operating cost is low, and equipment makes
It is long with the cycle, balance the relation of environmental protection, resource regeneration and financial cost well, realize to waste lubricating oil fully again
It is raw.
In a preferred embodiment, in step (a) waste oil pretreatment include carry out successively filtering, demulsification and
Backwash filter.
Specifically, step (a) includes:
(a1) filter:Strainer mesh number is used to be filtered for the filter of 60~100 mesh;
(a2) it is demulsified:The waste lubricating oil obtained after filtering is heated to 80~150 DEG C, desalted water is added in and demulsifier carries out
Washing demulsification after settling 5~8h, discharges bottom moisture and mechanical admixture;
(a3) backwash filter:The waste lubricating oil obtained after sedimentation enters in automatic backwashing filter, successively by 80 μ
M and 25 μm of strainer removes the impurity of larger particles and fine particle, and backwash filter is carried out in the case where temperature is 50~130 DEG C.
The pretreatment operation of the present invention is simple, and condition mitigates, and equipment investment is few, without complicated equipment, high treating effect,
Be conducive to improve production efficiency and reduce production cost.
In a preferred embodiment, step (b) includes:Pretreated waste lubricating oil is flashed, is removed
Traces of moisture and light component (100~360 DEG C of fractions), flash temperature are 100~260 DEG C, vacuum degree for -0.01~-
0.09Mpa。
In a preferred embodiment, step (c) includes:Waste lubricating oil after flash distillation enters propane extraction tower, with
Propane is extracted as extractant, wherein, the volume ratio (finish ratio) of waste lubricating oil and propane is 1:2~6, extraction temperature is
50~120 DEG C, extracting pressure is 3.5~4.3Mpa;
Materials at bottom of tower after the completion of extraction enters pitch propane recovery tower, recycles propane;
Tower top material enters supercritical propane recovery tower, and operating temperature is 100~150 DEG C, and pressure is 3.9~4.5Mpa,
Obtain intermediate product and propane;
Explanation is needed exist for, for pitch propane recovery tower for separating pitch and propane, concrete operations condition can root
According to conventional operate, supercritical propane recovery tower for separating intermediate product and propane, by pitch propane recovery tower and
The propane that supercritical propane recovery tower is collected into can be directly delivered in propane extraction tower again, and with recycling, reduction is produced into
This.
In the present invention, the typical but non-limiting volume ratio of waste lubricating oil and propane is 1:2、1:3、1:4、1:5 or 1:
6;It is 50 DEG C that extraction temperature is typical but non-limiting, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C, 95
DEG C, 100 DEG C, 105 DEG C, 110 DEG C, 115 DEG C or 120 DEG C;Extracting pressure it is typical but non-limiting for 3.5Mpa, 3.6Mpa,
3.7Mpa3.8Mpa, 3.9Mpa, 4.0Mpa, 4.1Mpa, 4.2Mpa or 4.3Mpa.
It is 100 DEG C that the operating temperature of supercritical propane recovery tower is typical but non-limiting, 105 DEG C, 110 DEG C, 115 DEG C,
120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C, 140 DEG C, 145 DEG C or 150 DEG C, pressure it is typical but non-limiting for 3.9Mpa,
4.0Mpa, 4.1Mpa, 4.2Mpa, 4.3Mpa, 4.4Mpa or 4.5Mpa.
The present invention is extracted under the conditions of relatively mild using propane extractant, without excessively high temperature and pressure (pressure
Power is in below 5MPa) etc. harsh process conditions, can in suitable operating condition and matched with other techniques
Enhance effect of extracting, effectively promote product quality, and avoid the pollutants such as acid sludge and waste water, environmental-friendly, the production cycle
Short, production efficiency is high.
In a preferred embodiment, step (d) includes:
(d1) intermediate product enters vacuum distillation tower, and operating temperature is 300~390 DEG C, and vacuum degree is -0.05
Waste lubricating oil is divided into multiple components by~-0.098Mpa according to boiling range and viscosity, is preferably 6 components;
(d2) intermediate product steams tower into thick, and operating temperature is 350~400 DEG C, vacuum degree for -0.01~-
0.099Mpa sloughs the impurity such as heavy constituent and carbon residue, obtains hydrogenation distillate.
By above-mentioned pretreatment, flash distillation, propane extraction, distillation etc. after operations, moisture, impurity, colloid in waste lubricating oil,
Asphalitine, heavy metal and additive etc. are removed substantially, meet requirement of the hydrofinishing to raw material, at this time can be by being hydrogenated with essence
System makes the removing of other undesirable components or saturation in waste lubricating oil, and then the purpose of waste lubricant oil regeneration.
In a preferred embodiment, the hydrogenation plant in step (e) includes three reactors being in series, successively
Include Ni-Co-Mo/Al for the first reactor of filling protective agent and metal remover, filling2O3The second of hydrogenation catalyst is anti-
It answers device and loads the 3rd reactor of antichlor.
In a preferred embodiment, step (e) includes hydrofinishing and post-refining, and device used includes phase
The hydrogenation plant and supplementary device of series connection, the hydrogenation plant include three reactors being in series, are followed successively by filling protective agent
First reactor, filling with metal remover include Ni-Co-Mo/Al2O3The second reactor of hydrogenation catalyst and filling
3rd reactor of antichlor, the supplementary device are to be in series and loaded including Ni-Co-Mo- with the 3rd reactor
Pd/Al2O34th reactor of aromatic hydrocarbon refining agent.
Explanation is needed exist for, three reactors or four reactors can be set in step (e), are preferably provided with four
Reactor can further promote oil quality.
The present invention does not do special restriction for protective agent, metal remover and antichlor, using commonly used in the art.
Such as the spherical Al-Ti-HY of macropore can be used as carrier in protective agent, Co-Mo is main active component;Metal remover can be adopted
It is carrier with mesoporous Raschig ring shape Si-Al oxides, Ni-Mo is main active component.Protective agent can be removed further
Glial component in waste oil reduces the accumulation of colloid, extends the service life of catalyst, and metal remover can further remove gold
Category, colloid, carbon deposit etc., and the alkene and aromatic hydrocarbons of saturation part mitigate the burden of follow up device, extend the cycle of operation of device.
Antichlor can make the chloride in waste oil be converted into hydrogen chloride, nitride converted for ammonia, can the burn into of anti-locking apparatus block
Deng ensureing the even running of device.
The hydrofinishing agent of the present invention employs the Ni-Co-Mo/Al of high activity2O3Catalyst, aromatic hydrocarbon refining agent use
The Ni-Co-Mo-Pd/Al of high activity2O3Catalyst helps to improve product quality, promotes product specification.
By hydrofinishing and post-refining, a large amount of sulphur nitrogen can be removed, saturation part condensed-nuclei aromatics is most of in raw material
Thrcylic aromatic hydrocarbon and double ring arene change into bicyclic and mononuclear aromatics, can obtain that condensation point is low, viscosity index (VI) is high, stability is good
Reclaimed Base Oil product so that the base oil product regenerated complies fully with the national standard of lube base oil.
In a preferred embodiment, step (e) includes:Hydrogenation distillate sequentially enters filling protection after decompression
The first reactor of agent and metal remover, filling include Ni-Co-Mo/Al2O3The second reactor of hydrogenation catalyst, filling are de-
3rd reactor of chlorine agent and filling include Ni-Co-Mo-Pd/Al2O34th reactor of aromatic hydrocarbon refining agent;
Wherein, the condition of hydrofinishing includes:Extraction temperature be 300~365 DEG C, pressure be 4~15Mpa, hydrogen oil volume
Than for 80~1500, liquid volume air speed is 0.1~1.5h- 1;
The condition of post-refining includes:Extraction temperature be 275~300 DEG C, pressure be 4~15Mpa, hydrogen to oil volume ratio 80
~1500, liquid volume air speed is 0.1~1.5h- 1。
In a preferred embodiment, the step of stripping is further included between step (f) and step (e), hydrogenation basis
Oil is into stripper, and under the conditions of temperature is 200~300 DEG C, the hydrogen sulfide and ammonia of removal hydrogenation reaction generation are stripped
Product.
In a preferred embodiment, step (f) includes:
(f1) stripped product enters decompression separation tower, and operating temperature is 100~300 DEG C, vacuum degree for -0.05~-
0.098Mpa removes light component caused by hydrocracking;
(f2) stripped product enters vacuum distillation tower, and operating temperature is 300~370 DEG C, vacuum degree for -0.05~-
0.098Mpa carries out fraction cutting according to boiling range and viscosity, obtains the hydrogenation regeneration oil product of different (viscosity) grades.
It should be noted that the temperature range of above-mentioned fraction cutting can be 305 ± 5 DEG C, 320 ± 5 DEG C, 350 ± 5 DEG C etc.
In a temperature or several temperature.The specific process parameter of vacuum rectification tower, such as reflux ratio and theoretical cam curve, can be by this
Field technology personnel are according to the adjusting of the progress routine such as difference of the inlet of material.
To sum up, method of the invention employs rational process route and condition, effectively removes various in waste lubricating oil
Undesirable components obtain reclaimed lubricating oil base oil best in quality, available for modulating various lube products, and operate letter
Single, easy to implement, environmental-friendly, the equipment cycle of operation, length was, it can be achieved that long period is continuously run.
Second aspect provides a kind of waste lubricant oil by hydrogenation refining system, includes successively:
Pretreatment unit, to remove the moisture and mechanical admixture in waste lubricating oil;
Flash tank, to remove remaining traces of moisture and light component in waste lubricating oil;
Propane extraction tower, pitch propane recovery tower and supercritical propane recovery tower, with remove the additive in waste lubricating oil,
Colloid, asphalitine and heavy metal, recycling propane and acquisition intermediate product;
Destilling tower, to remove the heavy constituent and carbon residue in intermediate product;
Hydrogenation plant to increase the saturated hydrocarbon content of lubricating oil and remove remaining impurity, obtains hydrogenated base oil;
And vacuum distillation tower, to isolate the base oil fractions in hydrogenated base oil, obtain hydrogenation regeneration oil product.
The hydrofinishing of waste lubricating oil is carried out, it can be achieved that waste lubricating oil using above system under the operating conditions described above
Fully regeneration improves the yield of Reclaimed Base Oil while Reclaimed Base Oil quality is improved, and the service cycle of device is long,
Equipment investment is few, and the service life of catalyst is long, advantageously reduces production cost while product quality and yield is improved, has
There is great commercial introduction to be worth.
It is understood that above-mentioned waste lubricant oil by hydrogenation refining system mainly includes above device, equipment, however it is not limited to
This, can also include relevant storage tank and accessory, and specific connection mode can refer to the prior art, and the present invention does not do this excessive
It limits.
With reference to specific embodiments and the drawings, the invention will be further described.
Embodiment 1
Fig. 1 shows waste lubricant oil by hydrogenation refining system structure diagram, as shown in Figure 1, the waste lubricant oil by hydrogenation
Refining system includes successively:
Pretreatment unit 1, to remove the moisture and mechanical admixture in waste lubricating oil;
Flash tank 2, to remove remaining traces of moisture and light component in waste lubricating oil;
Propane extraction tower 3, pitch propane recovery tower 5 and supercritical propane recovery tower 4, to remove the addition in waste lubricating oil
Agent, colloid, asphalitine and heavy metal, recycling propane and acquisition intermediate product;
Destilling tower 6, to remove the heavy constituent and carbon residue in intermediate product;
Hydrogenation plant and supplementary device to increase the saturated hydrocarbon content of lubricating oil and remove remaining impurity, obtain hydrogenation base
Plinth oil;Wherein, hydrogenation plant and supplementary device include the first reactor 7, second reactor 8, the 3rd reactor 9 being sequentially connected
With the 4th reactor 10;
Stripper 11, to remove the hydrogen sulfide and ammonia of hydrogenation reaction generation;
With vacuum distillation tower 12, to isolate the base oil fractions in hydrogenated base oil, hydrogenation regeneration oil product is obtained.
A kind of waste lubricant oil by hydrogenation process for purification, comprises the following steps:
(a) waste oil pre-processes:Waste lubricating oil is dehydrated and is cleaned pretreatment;
(a1) filter:Strainer mesh number is used to be filtered for the filter of 80 mesh;
(a2) it is demulsified:The waste lubricating oil obtained after filtering is heated to 80 DEG C, desalted water is added in and demulsifier is washed
Demulsification after settling 5h, discharges bottom moisture and mechanical admixture;
(a3) backwash filter:The waste lubricating oil obtained after sedimentation enters in automatic backwashing filter, successively by 80 μ
M and 25 μm of strainer removes the impurity of larger particles and fine particle, and backwash filter is carried out in the case where temperature is 50 DEG C;
(b) flash:Pretreated waste lubricating oil is flashed, removes (100~360 DEG C of traces of moisture and light component
Fraction), flash temperature is 100 DEG C, and vacuum degree is -0.01Mpa;
(c) propane extracts:Waste lubricating oil after flash distillation enters propane extraction tower, is extracted using propane as extractant,
Wherein, finish ratio is 1:2, extraction temperature is 50 DEG C, extracting pressure 3.5Mpa;
Materials at bottom of tower after the completion of extraction enters pitch propane recovery tower, recycles propane;Tower top material enters overcritical third
Alkane recovery tower, operating temperature are 100 DEG C, pressure 3.9Mpa, obtain intermediate product and propane;
(d) distill:Distillation processing is carried out to intermediate product, to slough heavy constituent and carbon residue, obtains hydrogenation distillate;
(d1) intermediate product enters vacuum distillation tower, and operating temperature is 300 DEG C, and vacuum degree is -0.05Mpa, according to boiling range
Waste lubricating oil is divided into 6 components with viscosity;
(d2) intermediate product steams tower into thick, and operating temperature is 350 DEG C, and vacuum degree is -0.01Mpa, slough heavy constituent and
The impurity such as carbon residue obtain hydrogenation distillate;
(e) hydrofinishing:Hydrogenation distillate sequentially enters the first reaction of filling protective agent and metal remover after decompression
Device, filling include Ni-Co-Mo/Al2O3The second reactor of hydrogenation catalyst, the 3rd reactor and dress for loading antichlor
It fills out including Ni-Co-Mo-Pd/Al2O34th reactor of aromatic hydrocarbon refining agent obtains hydrogenated base oil;
Wherein, the condition of hydrofinishing includes:Extraction temperature is 300 DEG C, pressure 4Mpa, hydrogen to oil volume ratio 80, liquid
Body volume space velocity is 0.1h- 1;The condition of post-refining includes:Extraction temperature is 275 DEG C, pressure 4Mpa, and hydrogen to oil volume ratio is
80, liquid volume air speed is 0.1h- 1;
(f) strip:Hydrogenated base oil enters stripper, under the conditions of temperature is 200 DEG C, the sulphur of removal hydrogenation reaction generation
Change hydrogen and ammonia, obtain stripped product;
(g1) stripped product enters decompression separation tower, and operating temperature is 100 DEG C, and vacuum degree is -0.05Mpa, and removal is hydrogenated with
Light component caused by cracking;
(g2) stripped product enters vacuum distillation tower, and operating temperature is 300 DEG C, and vacuum degree is -0.05Mpa, is hydrogenated with
Regenerate oil product.
The yield of the regeneration oil product of gained is 85.4% in the present embodiment.
Embodiment 2
A kind of waste lubricant oil by hydrogenation process for purification, comprises the following steps:
(a) waste oil pre-processes:Waste lubricating oil is dehydrated and is cleaned pretreatment;
(a1) filter:Strainer mesh number is used to be filtered for the filter of 80 mesh;
(a2) it is demulsified:The waste lubricating oil obtained after filtering is heated to 150 DEG C, desalted water is added in and demulsifier is washed
Demulsification after settling 8h, discharges bottom moisture and mechanical admixture;
(a3) backwash filter:The waste lubricating oil obtained after sedimentation enters in automatic backwashing filter, successively by 80 μ
M and 25 μm of strainer removes the impurity of larger particles and fine particle, and backwash filter is carried out in the case where temperature is 130 DEG C;
(b) flash:Pretreated waste lubricating oil is flashed, removes (100~360 DEG C of traces of moisture and light component
Fraction), flash temperature is 260 DEG C, and vacuum degree is -0.09Mpa;
(c) propane extracts:Waste lubricating oil after flash distillation enters propane extraction tower, is extracted using propane as extractant,
Wherein, finish ratio is 1:3, extraction temperature is 120 DEG C, extracting pressure 4.3Mpa;
Materials at bottom of tower after the completion of extraction enters pitch propane recovery tower, recycles propane;Tower top material enters overcritical third
Alkane recovery tower, operating temperature are 150 DEG C, pressure 4.5Mpa, obtain intermediate product and propane;
(d) distill:Distillation processing is carried out to intermediate product, to slough heavy constituent and carbon residue, obtains hydrogenation distillate;
(d1) intermediate product enters vacuum distillation tower, and operating temperature is 390 DEG C, and vacuum degree is -0.098Mpa, according to evaporating
Waste lubricating oil is divided into 6 components by journey and viscosity;
(d2) intermediate product steams tower into thick, and operating temperature is 400 DEG C, and vacuum degree is -0.099Mpa, sloughs heavy constituent
Distillate is hydrogenated with impurity, acquisitions such as carbon residues;
(e) hydrofinishing:Hydrogenation distillate sequentially enters the first reaction of filling protective agent and metal remover after decompression
Device, filling include Ni-Co-Mo/Al2O3The second reactor of hydrogenation catalyst, the 3rd reactor and dress for loading antichlor
It fills out including Ni-Co-Mo-Pd/Al2O34th reactor of aromatic hydrocarbon refining agent obtains hydrogenated base oil;
Wherein, the condition of hydrofinishing includes:Extraction temperature is 365 DEG C, pressure 15Mpa, hydrogen to oil volume ratio 1500,
Liquid volume air speed is 1.5h- 1;The condition of post-refining includes:Extraction temperature is 300 DEG C, pressure 15Mpa, hydrogen oil volume
Than for 1500, liquid volume air speed is 1.5h- 1;
(f) strip:Hydrogenated base oil enters stripper, under the conditions of temperature is 300 DEG C, the sulphur of removal hydrogenation reaction generation
Change hydrogen and ammonia, obtain stripped product;
(g1) stripped product enters decompression separation tower, and operating temperature is 300 DEG C, and vacuum degree is -0.098Mpa, and removal adds
Light component caused by hydrogen cracking;
(g2) stripped product enters vacuum distillation tower, and operating temperature is 370 DEG C, and vacuum degree is -0.098Mpa, is added
Hydrogen regenerates oil product.
The yield of the regeneration oil product of gained is 88.2% in the present embodiment.
Embodiment 3
A kind of waste lubricant oil by hydrogenation process for purification, comprises the following steps:
(a) waste oil pre-processes:Waste lubricating oil is dehydrated and is cleaned pretreatment;
(a1) filter:Strainer mesh number is used to be filtered for the filter of 80 mesh;
(a2) it is demulsified:The waste lubricating oil obtained after filtering is heated to 120 DEG C, desalted water is added in and demulsifier is washed
Demulsification after settling 7h, discharges bottom moisture and mechanical admixture;
(a3) backwash filter:The waste lubricating oil obtained after sedimentation enters in automatic backwashing filter, successively by 80 μ
M and 25 μm of strainer removes the impurity of larger particles and fine particle, and backwash filter is carried out in the case where temperature is 100 DEG C;
(b) flash:Pretreated waste lubricating oil is flashed, removes (100~360 DEG C of traces of moisture and light component
Fraction), flash temperature is 200 DEG C, and vacuum degree is -0.05Mpa;
(c) propane extracts:Waste lubricating oil after flash distillation enters propane extraction tower, is extracted using propane as extractant,
Wherein, finish ratio is 1:4, extraction temperature is 95 DEG C, extracting pressure 4.0Mpa;
Materials at bottom of tower after the completion of extraction enters pitch propane recovery tower, recycles propane;Tower top material enters overcritical third
Alkane recovery tower, operating temperature are 130 DEG C, pressure 4.3Mpa, obtain intermediate product and propane;
(d) distill:Distillation processing is carried out to intermediate product, to slough heavy constituent and carbon residue, obtains hydrogenation distillate;
(d1) intermediate product enters vacuum distillation tower, and operating temperature is 370 DEG C, and vacuum degree is -0.08Mpa, according to boiling range
Waste lubricating oil is divided into 6 components with viscosity;
(d2) intermediate product steams tower into thick, and operating temperature is 380 DEG C, and vacuum degree is -0.08Mpa, slough heavy constituent and
The impurity such as carbon residue obtain hydrogenation distillate;
(e) hydrofinishing:Hydrogenation distillate sequentially enters the first reaction of filling protective agent and metal remover after decompression
Device, filling include Ni-Co-Mo/Al2O3The second reactor of hydrogenation catalyst, the 3rd reactor and dress for loading antichlor
It fills out including Ni-Co-Mo-Pd/Al2O34th reactor of aromatic hydrocarbon refining agent obtains hydrogenated base oil;
Wherein, the condition of hydrofinishing includes:Extraction temperature is 350 DEG C, pressure 12Mpa, hydrogen to oil volume ratio 1000,
Liquid volume air speed is 1.2h- 1;The condition of post-refining includes:Extraction temperature is 290 DEG C, pressure 12Mpa, hydrogen oil volume
Than for 800, liquid volume air speed is 1.1h- 1;
(f) strip:Hydrogenated base oil enters stripper, under the conditions of temperature is 280 DEG C, the sulphur of removal hydrogenation reaction generation
Change hydrogen and ammonia, obtain stripped product;
(g1) stripped product enters decompression separation tower, and operating temperature is 220 DEG C, and vacuum degree is -0.06Mpa, and removal is hydrogenated with
Light component caused by cracking;
(g2) stripped product enters vacuum distillation tower, and operating temperature is 350 DEG C, and vacuum degree is -0.06Mpa, is hydrogenated with
Regenerate oil product.
The yield of the regeneration oil product of gained is 92.6% in the present embodiment.
Embodiment 4
A kind of waste lubricant oil by hydrogenation process for purification, comprises the following steps:
(a) waste oil pre-processes:Waste lubricating oil is dehydrated and is cleaned pretreatment;
(a1) filter:Strainer mesh number is used to be filtered for the filter of 80 mesh;
(a2) it is demulsified:The waste lubricating oil obtained after filtering is heated to 100 DEG C, desalted water is added in and demulsifier is washed
Demulsification after settling 6h, discharges bottom moisture and mechanical admixture;
(a3) backwash filter:The waste lubricating oil obtained after sedimentation enters in automatic backwashing filter, successively by 80 μ
M and 25 μm of strainer removes the impurity of larger particles and fine particle, and backwash filter is carried out in the case where temperature is 80 DEG C;
(b) flash:Pretreated waste lubricating oil is flashed, removes (100~360 DEG C of traces of moisture and light component
Fraction), flash temperature is 150 DEG C, and vacuum degree is -0.04Mpa;
(c) propane extracts:Waste lubricating oil after flash distillation enters propane extraction tower, is extracted using propane as extractant,
Wherein, finish ratio is 1:5, extraction temperature is 70 DEG C, extracting pressure 3.8Mpa;
Materials at bottom of tower after the completion of extraction enters pitch propane recovery tower, recycles propane;Tower top material enters overcritical third
Alkane recovery tower, operating temperature are 110 DEG C, pressure 4.1Mpa, obtain intermediate product and propane;
(d) distill:Distillation processing is carried out to intermediate product, to slough heavy constituent and carbon residue, obtains hydrogenation distillate;
(d1) intermediate product enters vacuum distillation tower, and operating temperature is 320 DEG C, and vacuum degree is -0.05Mpa, according to boiling range
Waste lubricating oil is divided into 6 components with viscosity;
(d2) intermediate product steams tower into thick, and operating temperature is 360 DEG C, and vacuum degree is -0.04Mpa, slough heavy constituent and
The impurity such as carbon residue obtain hydrogenation distillate;
(e) hydrofinishing:Hydrogenation distillate sequentially enters the first reaction of filling protective agent and metal remover after decompression
Device, filling include Ni-Co-Mo/Al2O3The second reactor of hydrogenation catalyst, the 3rd reactor and dress for loading antichlor
It fills out including Ni-Co-Mo-Pd/Al2O34th reactor of aromatic hydrocarbon refining agent obtains hydrogenated base oil;
Wherein, the condition of hydrofinishing includes:Extraction temperature is 320 DEG C, pressure 6Mpa, hydrogen to oil volume ratio 200, liquid
Body volume space velocity is 0.5h- 1;The condition of post-refining includes:Extraction temperature is 220 DEG C, pressure 6Mpa, and hydrogen to oil volume ratio is
300, liquid volume air speed is 0.5h- 1;
(f) strip:Hydrogenated base oil enters stripper, under the conditions of temperature is 220 DEG C, the sulphur of removal hydrogenation reaction generation
Change hydrogen and ammonia, obtain stripped product;
(g1) stripped product enters decompression separation tower, and operating temperature is 220 DEG C, and vacuum degree is -0.05Mpa, and removal is hydrogenated with
Light component caused by cracking;
(g2) stripped product enters vacuum distillation tower, and operating temperature is 320 DEG C, and vacuum degree is -0.05Mpa, is hydrogenated with
Regenerate oil product.
The yield of the regeneration oil product of gained is 93.8% in the present embodiment.
Embodiment 5
A kind of waste lubricant oil by hydrogenation process for purification, with differing only in for embodiment 4:
(c) propane extracts:Waste lubricating oil after flash distillation enters propane extraction tower, is extracted using propane as extractant,
Wherein, finish ratio is 1:6, extraction temperature is 85 DEG C, extracting pressure 3.85Mpa;
Materials at bottom of tower after the completion of extraction enters pitch propane recovery tower, recycles propane;Tower top material enters overcritical third
Alkane recovery tower, operating temperature are 125 DEG C, pressure 4.25Mpa, obtain intermediate product and propane;
The yield of the regeneration oil product of gained is 94.3% in the present embodiment.
Embodiment 6
A kind of waste lubricant oil by hydrogenation process for purification, with differing only in for embodiment 4:
(e) condition of hydrofinishing includes:Extraction temperature is 305 DEG C, pressure 8.5Mpa, hydrogen to oil volume ratio 950, liquid
Body volume space velocity is 0.9h- 1;The condition of post-refining includes:Extraction temperature is 235 DEG C, pressure 7.5Mpa, hydrogen to oil volume ratio
For 150, liquid volume air speed is 0.7h- 1;
The yield of the regeneration oil product of gained is 90.5% in the present embodiment.
Comparative example 1
A kind of waste lubricant oil by hydrogenation process for purification, with differing only in for embodiment 4:
Propane extraction in step (c) is replaced with into absorption, adsorbent uses alumina adsorbant:
The yield of the regeneration oil product of gained is 75.2% in this comparative example;After tested, the reclaimed oil that this comparative example obtains
Viscosity index (VI) for 100, acid value 0.022mg/g, total metal content 105ppm.
Comparative example 2
A kind of waste lubricant oil by hydrogenation process for purification, with differing only in for embodiment 4:
Omit step (c);
The yield of the regeneration oil product of gained is 66.4% in this comparative example;After tested, the reclaimed oil that this comparative example obtains
Viscosity index (VI) for 98, acid value 0.026mg/g, total metal content 138ppm.
Comparative example 3
A kind of waste lubricant oil by hydrogenation process for purification, with differing only in for embodiment 4:
Omit the first reactor and the 3rd reactor in step (e).
The yield of the regeneration oil product of gained is 77.6% in this comparative example;After tested, the reclaimed oil that this comparative example obtains
Viscosity index (VI) for 102, acid value 0.032mg/g, total metal content 185ppm.
In addition, comparative example 1-3 is in process of production, due to not filled to the removing of heavy metal, the colloid in waste lubricating oil etc.
Divide, add the load of the processes such as distillation, hydrofinishing, the easy coking of equipment be easy to cause the blocking of device, equipment operation week
Phase is short, and catalyst service life is shorter, reduces device traveling comfort, and production efficiency is relatively low.
The feedstock property of waste lubricating oil used in above-described embodiment and comparative example is as shown in table 1.
1 waste lubricating oil feedstock property of table
The regeneration oil product obtained by each embodiment is subjected to quality index test respectively, test result is as shown in table 2.
2 quality of reclaimed index of table
Wherein, waste lubricating oil raw material and the test method of gained reclaimed oil are:According to standard GB/T/T8929-2006
Water content is tested, kinematic viscosity is tested according to standard GB/T/T265, Saybolt color is measured according to ASTMD156, according to
Standard GB/T/T1995 tested viscosity indexes tests open flash point according to standard GB/T/T3536, according to standard GB/T/
T3535 tests pour point, and acid value is tested according to standard GB/T/T7304, according to standard GB/T/T2013 test densitys, according to
SH/T0193 tests lubricating oil oxidation stability, according to ASTM-D6595-17 aes determinations metal and impurity
Test method measure tenor and impurity content, saturated hydrocarbon content measures (embodiment and comparative example using gas chromatography
The test method of gained reclaimed oil is identical).
As can be seen from Table 2, the quality for the reclaimed oil that 1-6 of the embodiment of the present invention is provided is slightly different, but each reclaimed oil
Quality index can meet lubricating oil general basic oil ga(u)ge alignment request, available for various lube products are modulated, especially implement
The regeneration oil product overall target that example 3 obtains is the most excellent.
Meanwhile by above it can also be seen that regeneration oil quality provided by the invention is provided again better than comparative example 1-3
The quality of raw base oil especially in the indexs such as viscosity index (VI), total metal content, has superior effect;The present invention simultaneously
The yield for the reclaimed oil that embodiment 1-6 is provided is also apparently higher than the yield of the comparative example 1-3 reclaimed oils provided, by this hair
The hydrofinishing process of bright offer, can not only promote the quality and yield of reclaimed oil, and can also lifting means operation stabilization
Property, avoid impurity equipment is caused coking etc. damage equipment the phenomenon that, prevent system congestion, extend equipment the cycle of operation and urge
The service life of agent, effectively increases production efficiency.
Finally it should be noted that:The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent
Pipe is described in detail the present invention with reference to foregoing embodiments, it will be understood by those of ordinary skill in the art that:Its according to
Can so modify to the technical solution recorded in foregoing embodiments either to which part or all technical characteristic into
Row equivalent substitution;And these modifications or replacement, the essence of appropriate technical solution is not made to depart from various embodiments of the present invention technology
The scope of scheme.