CN106336939A - Refining technique of base oil regenerated from used lubrication oil - Google Patents

Refining technique of base oil regenerated from used lubrication oil Download PDF

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Publication number
CN106336939A
CN106336939A CN201610749463.7A CN201610749463A CN106336939A CN 106336939 A CN106336939 A CN 106336939A CN 201610749463 A CN201610749463 A CN 201610749463A CN 106336939 A CN106336939 A CN 106336939A
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oil
solvent
refining
distillation
gas
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康兴永
岳安涛
李刚
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Ji'nan Promise Renewable Resources Co Ltd
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Ji'nan Promise Renewable Resources Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning
    • C10M175/0025Working-up used lubricants to recover useful products ; Cleaning by thermal processes
    • C10M175/0033Working-up used lubricants to recover useful products ; Cleaning by thermal processes using distillation processes; devices therefor
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning
    • C10M175/005Working-up used lubricants to recover useful products ; Cleaning using extraction processes; apparatus therefor
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning
    • C10M175/0058Working-up used lubricants to recover useful products ; Cleaning by filtration and centrifugation processes; apparatus therefor

Abstract

Disclosed is a refining technique of base oil regenerated from used lubrication oil, and the refining technique comprises the following steps of 1, removing solid waste, which includes removing solid waste from used lubrication oil by centrifugation; 2, solvent pretreatment, which includes extracting mixed impurities and moisture through a solvent and obtaining raw oil after removing upper oil; 3, flocculation treatment, which includes turning mixtures obtained from step 2 into a mixture of flocculation; 4, atomospheric distillation; 5, carrying out reduced pressure distillation; 6, carrying out rectification; 7, solvent refining: putting oil produced from a rectifying column into a treatment tank and when the height of the oil level in the treatment tank reaches 65%-75% of the height of the treatment tank, adding by mass 10%-40% of 1-Methyl-2-pyrrolidinone, and carrying out solvent refining. The refining technique of base oil regenerated from used lubrication oil has the advantages of low investment and high yield efficiency, meanwhile, the refining technique accords with the requirement of environmental protection, reduces vacuum residuum by 15%, improves product yield, facilitates the overhauling of equipment, prolongs the production period, largely improves production efficiency and appearance quality of minus line oil, and helps to obtain high quality regenerated base oil.

Description

A kind of refining process of producing base oil by regenerating waste lubricating oil
Technical field
The present invention relates to a kind of for the refining process by Reclaimed Base Oil in waste lubricating oil, belong to waste lubricant oil regeneration skill Art field.
Background technology
Domestic waste lubricating oil refines base oil technique, how with normal pressure plug, sulfuric acid treatment one milk of lime carclazyte work, its work Skill is complicated to fall behind, and goods and materials waste, and environmental pollution is serious.The regeneration of external waste lubricating oil is how based on hydrogenation technique.
The note of " waste lubricant oil regeneration " third edition according in August, 2000 second printing distribution of Sinopec publishing house Carry, abroad adopt film distilled carclazyte technique, this technique products obtained therefrom base oil yield is only 65%, light oil 7%, and product is comprehensive Close yield 72%, and byproduct residual oil discharge rate is up to 28%, more containing lubricating oil component in residual oil, account for the 20% of residual oil amount Left and right, this kind of residual oil added value is very low, belongs to hazardous waste, and residual oil amount is excessive.
Because lubricating oil creates greasy filth and deposit in use, generates acids, corrosion and retrogradation etc. occur, because All suitable antioxidant levels are defined according to specific use requirement in this most lubricating oil specification, that is, oxidation peace Qualitative, so that ability to work under extremely exacting terms for the service life of lubricating oil is improved.20 century 70s Since, because scientific and technological continuous development and progress makes China to the usage amount of oil increasing year by year, and then the yield of oil Also aggravate continuous, and high-quality crude is fewer and feweri, the crude oil of the output such as Daqing oil field, Shengli Oil Field, Karamay oilfield And the crude oil of external import, its acid number is higher to be had on its price and following process etc. significantly affects.Therefore oil product and Waste oil deacidifying process is imperative.
Acidic materials in lube base oil are all the compounds of some non-hydrocarbons, comprising: sulfur-containing compound, nitrogen Compound and oxygenatedchemicals.Mainly aliphatic acid, aphthenic acids, aromatic acid, phenol, mercaptan, inorganic acid etc., are referred to as petroleum acids, Account for the 1%-2% of crude quality.The quality of wherein aphthenic acids accounts for the 90% about of petroleum acids gross mass, so aphthenic acids is almost Become the synonym of petroleum acids, that is, topmost Acid bearing-oxygen compound in waste lubricating oil.Aphthenic acids is a kind of viscosity liquid State compound, color is in faint yellow to amber, is practically insoluble in water, is soluble in organic solvent, in oil product, this is also aphthenic acids The reason be difficult to abjection.
The harm of lubricating oil distillate middle acid substance: aphthenic acids has certain corrosivity, easily makes equipment and pipeline Corrosion is even revealed.In process, the metal erosion being caused by aphthenic acids in words to crude oil containing aphthenic acids there is.Ring Alkanoic acid corrosion process is the property of corrosive medium and the coefficient result of scouring intensity of fluid, in naphthenic acid corrosion process In, temperature, acid number, flow velocity, time etc. are the key factors to metal erosion for the aphthenic acids, seriously corroded will impact device just Often operate, or even jeopardize production and personal safety, cause economic loss and pollute environment, in addition also affect the peace of oil product Qualitative.
Chinese patent literature cn102373108a is disclosed " a kind of process of producing base oil by regenerating waste lubricating oil ", is logical Cross waste lubricating oil pretreatment, thin film evaporation, molecular clock, clay-filtered and flash liberation processing step are realized.
Cn103820200a is disclosed " a kind of technique by producing base oil by regenerating waste lubricating oil ", including 1) waste lubricating oil is existed Under conditions of being not less than 60 DEG C, sedimentation, centrifugation, are then heated to 100-110 DEG C and are evaporated, obtain pre-treated oil;2) By be not less than 60 DEG C of described pre-treated oil successively through fenestra be 1-3 μm, 0.1-1 μm and the three-stage ceramic film less than 0.1 μm After filtration, carry out being not less than 200 DEG C of thin film evaporation;3) the remaining oil plant after thin film evaporation is carried out three-level molecule short distance to steam Evaporate, collect distillations at different levels.
Cn103849454a disclosed " a kind of device by producing base oil by regenerating waste lubricating oil ", including settling tank, centrifuge, Heating evaporation device, three-stage ceramic membrane separator, thin film evaporator and three-level molecule short-distance distiller, settling tank and centrifuge phase Even, centrifuge is connected with heating evaporation device, and heating evaporation device oil-out is connected with first order ceramic membrane separation device oil-in, phase Adjacent ceramic membrane separation device is connected with oil-in by edible vegetable oil outlet, and third level ceramic membrane separation device edible vegetable oil exports and thin film evaporation Device oil-in is connected, and thin film evaporator oil-out is connected with first order molecule short-distance distiller oil-in, and adjacent molecule is short Journey distiller is connected with oil-in by heavy oil outlet, the fenestra of one to three-stage ceramic membrane separator be followed successively by more than 1 μm, 0.1-1 μm and 0.01-0.1 μm.
The technology of above-mentioned producing base oil by regenerating waste lubricating oil although producing base oil by regenerating waste lubricating oil can be made, but therein Acidic materials are not all effectively removed, and there is acid corrosion phenomenon, also do not meet environmental requirement,
Content of the invention
The deficiency that the present invention exists according to waste lubricating oil characteristic and the basic oil tech of existing waste lubricating oil refining, provides one kind Invest low, high income, meet environmental requirement, be obtained in that the refining of the producing base oil by regenerating waste lubricating oil of high-quality Reclaimed Base Oil Technique.
The refining process of the producing base oil by regenerating waste lubricating oil of the present invention, including abjection solid waste, solvent pre-treatment, flocculation Process, air-distillation, vacuum distillation, rectifying and solvent refining, details are provided below:
(1) deviate from solid waste:
Centrifugation removes the solid waste in the waste lubricating oil collected;
(2) solvent pre-treatment:
No. 120 solvent naphthas and the methyl tertiary butyl ether(MTBE) ratio of 1:1~1:5 in mass ratio are mixed, makes mixing molten Agent, waste lubricating oil and the mixed solvent ratio of 1:1.5~1:2 in mass ratio are mixed, stirring, and standing isolates mixing Impurity and moisture;Take upper strata oil, after removing the solvent in the oil of upper strata, obtain feedstock oil;
(3) flocculation treatment:
In feedstock oil, the ratio of 1:0.5~1:1 injects flocculant in mass ratio, simultaneously in mass ratio 1 in feedstock oil: The ratio of 0.01~1:0.05 adds sodium hydroxide solution or potassium hydroxide solution, stirs 0.5 hour -2 hours, becomes flocculation mixed Compound;
Described sodium hydroxide solution or potassium hydroxide solution press NaOH or potassium hydroxide with water quality than 1:4~5:8 Proportions;
(4) air-distillation:
Flocculated mixture, in 110 DEG C of -150 DEG C of the pre-heat treatment, obtains top light oil gas and bottom heavy constituent;Top light oil gas Enter atmospheric flash tower and carry out Oil-gas Separation, as fuel after the gas isolated is condensed, the light oil distributing reclaims profit With;Bottom heavy constituent entrance atmospheric evaporation device is heated to 260 DEG C -340 DEG C and carries out air-distillation;
Described Oil-gas Separation is to carry out when atmospheric flash tower internal upper part temperature is 160 DEG C to 220 DEG C.
In described atmospheric evaporation device, the Liquid level of heavy constituent is the 30%~70% of atmospheric evaporation device capacity.
(5) vacuum distillation:
The oil that air-distillation goes out carries out vacuum flashing fractionation first, obtains top oil gas and bottom oil ingredient, top Oil gas is directly entered rectifying column fractionation, and oil ingredient enters decompression evaporator and carries out scraping Membrane Materials, and the oil gas that knifing distills out is continuous Ascend into rectifying column;
(6) rectifying:
The oil gas that vacuum distillation goes out enters rectifying column, separates residual oil;The oil that rectifying column fractionates out when 120 DEG C -150 DEG C, By the mass ratio of oil and carclazyte 5:0.6~5:1, oil adds carclazyte, is circulated 15 minutes -45 minutes by stripper, remove The peculiar smell that distillation produces;
(7) solvent refining:
In rectifying column, the oil of output enters in treatment tank, when refined hand-dipping liquid level is in refined tankage size 65%- When 75%, the nmp (n- methyl pyrrolidone) of oil mass quality 10%-40% is added to carry out solvent refining.
Solvent refining is first the oil in treatment tank to be cooled to 100 DEG C -120 DEG C, then stirs, and carries out solvent extraction suction Attached.
Oil after refined is stored in finished pot after filter filtration.
The present invention invests low, high income, meets environmental requirement, has the following characteristics that
1. waste lubricating oil solvent isolates most moisture and inorganic impurity, it is to avoid when air-distillation and vacuum distillation Because temperature produce coking, decompression residuum reduce 15%, improve product yield, yield between 70~95%, beneficial to equipment Maintenance, extends the production cycle, substantially increases production efficiency, make product maximizing the benefits.
2. the detached job of vacuum flasher and vacuum rectification tower, entrainment when effectively avoiding flash distillation, rectifying column The more efficient fractionation carrying out each section of cut, rectifying column is difficult coking, has ensured the high vacuum of rectifying column.
3. carry out solvent refining, substantially increase the presentation quality improving product oil, improve product oil oxidative safety Property, obtain high-quality Reclaimed Base Oil.
Brief description
Fig. 1 is the process flow diagram of the present invention.
Fig. 2 is stage of rectification process flow diagram in the present invention.
Fig. 3 is boiler heating operation schematic diagram in the present invention.
Fig. 4 is refined oil temperature-fall period schematic diagram in the present invention.
Specific embodiment
The process chart being given as Fig. 1 and Fig. 2, the refining process of producing base oil by regenerating waste lubricating oil of the present invention includes deviating from Solid waste, solvent pre-treatment, flocculation treatment, air-distillation, vacuum distillation, rectifying and solvent refining stage, detailed process is such as Lower described.
(1) deviate from solid waste
By the waste lubricating oil collected injection supercentrifuge, centrifugation removes the solid waste inside waste lubricating oil, to obtain Without the waste lubricating oil of solid impurity, effectively prevent after it enters firing equipment and produce coking material.
(2) solvent pre-treatment
No. 120 solvent naphthas and the methyl tertiary butyl ether(MTBE) ratio of 1:1~1:5 in mass ratio are mixed, makes mixing molten Agent, waste lubricating oil and the mixed solvent ratio of 1:1.5~1:2 in mass ratio are mixed, and stir 0.5-1 hour, stand 5-8 Little layered, isolates poly-doped impurity and moisture;Take upper strata oil, removed in the oil of upper strata by methods such as existing temperature-pressure extractions Solvent, obtain feedstock oil.
(3) flocculation treatment
In feedstock oil, the ratio of 1:0.5~1:1 injects flocculant in mass ratio, simultaneously in mass ratio 1 in feedstock oil: The ratio of 0.01~1:0.05 adds sodium hydroxide solution or potassium hydroxide solution, stirs 0.5 hour -2 hours, becomes flocculation mixed Compound.
Described sodium hydroxide solution or potassium hydroxide solution press NaOH or potassium hydroxide with water quality than 1:4~5:8 Proportions.
Neutralize carboxyl in oil acid molecule using NaOH or potassium hydroxide, realize depickling, effective control aphthenic acids Corrosion phenomenon, this proportioning is best suitable for being applied to the refining of waste oil regeneration base oil.
(4) air-distillation
Flocculated mixture is in 110 DEG C of -150 DEG C of the pre-heat treatment, the top light oil gas obtaining and bottom heavy constituent;Top light oil Gas enters atmospheric flash tower and carries out Oil-gas Separation, sends into boiler combustion, the light oil distributing after the gas isolated is condensed It is recycled in light oil tank, in case boiler auxiliary combustion;Bottom heavy constituent entrance atmospheric evaporation device is heated to 260 DEG C -340 DEG C often to be carried out Pressure distillation.
As shown in Fig. 2 specific operation process is as described below.
1. it is opened for water pump and the vacuum system (the big vacuum group in Fig. 2 and little vacuum group) of gas fired-boiler water supply, vacuum System total valve is opened to 1/3, opens fore pump, notes observing vacuum system pressure gauge, treats that vacuum pressure is 0.09 MPa, By vacuum system open to automatically (now, vavuum pump can according to one-level, two grades, three-level, level Four start-up mode automatically turn on), see Examine system vacuum, in about 20 minutes systems, vacuum reaches requirement for 0.1 MPa.
2. open gas fired-boiler (referring to Fig. 3), fused salt (medium of heating) valve is all turned on, treats that in burner hearth, temperature is extremely 260 DEG C of unlatching boiler lava pumps (because if fire box temperature does not reach more than 260, fused salt fragile boiler inner coil pipe, occur stifled Plug coking), fused salt is heated up to 400 DEG C.Now note observing automatic boiler control and temperature display system, treat fused salt tank temperature To 400 DEG C, gas furnace robot control system(RCS) is opened fully automatic mode.
The steam of gas fired-boiler runs as shown in figure 3, providing heat for atmospheric evaporation device, decompression evaporator and stripper.
3. carry out air-distillation after flocculated mixture being pre-processed
Open the valve that oils, open oiling pump, the flocculated mixture that step (3) coagulation is in harmonious proportion first passes through gas-fired boiler The flue heat exchange of stove, the temperature using gas boiler flue is preheated for the first time, 110 DEG C -150 DEG C of preheating temperature.Now can produce Raw a part of on-condensible gas, this part on-condensible gas is entered atmospheric flash tower by pumping, carries out Oil-gas Separation process.
It should be noted that observing temperature change after entering atmospheric flash tower, observe atmospheric flash tower upper temp and temperature of lower, When upper temp is to 160 DEG C to 220 DEG C, it is the optimal temperature of Oil-gas Separation, enter after the condensation of on-condensible gas condensed device Normal pressure water sealed tank, is entered in gas fired-boiler by normal pressure water sealed tank and burns, to reach combustion-supporting purpose.Upper temp 160 DEG C- When 220 DEG C, temperature of lower can be opened light oil reflux pump, atmospheric flash tower shunted in 220 DEG C to 300 DEG C this intervals The light oil going out is recycled in light oil tank, in case combustion-supporting.
Bottom heavy constituent entrance atmospheric evaporation device in atmospheric flash tower is heated to 260 DEG C -340 DEG C and carries out air-distillation.
Due to waste lubricating oil characteristic and property proterties it is not necessary to as processing crude oil, through many experiments, normal pressure Evaporimeter design temperature is the most reasonable at 260 DEG C -340 DEG C, carries out atmospheric pressure low temperature distillation at this temperature, had both deviate from colloid Pitch, is avoided that the equipment loss that in evaporimeter, coking causes again, and the quality just steaming base oil can also be guaranteed, does not change basis The physical characteristic of oil, viscosity index (VI).
Operation has to comply with technological requirement safety requirements and environmental requirement, and temperature control is the pass of waste oil regeneration base oil Key, in units of per hour, observes oil temperature change, up and down scope is regime values within 10 DEG C, such as less than 10 DEG C with On, to check whether normal pressure lava pump goes wrong, whether gas furnace occurs shutting down, because the upper limit controls temperature to be locked as 340 DEG C it is therefore necessary to observe 285 DEG C of normal temperature and 260 DEG C of lower limit temperature.
The height of atmospheric evaporation device liquid level has important shadow to the effect of next process and entrance reduced-pressure flash tank Ring.Through many experiments, in atmospheric evaporation device, the Liquid level of heavy constituent is managed the most the 30%~70% of atmospheric evaporation device capacity Think.
The oil that heavy constituent obtains after air-distillation carries out vacuum distillation again,
(5) vacuum distillation
The oil obtaining after air-distillation, initially enters vacuum flasher, and the top oil gas obtaining in vacuum flasher is straight Tap into into rectifying column, oil ingredient then enters decompression evaporator heating, separates residual oil, separates cut.Details are provided below.
To 285 DEG C and after 30 minutes, open decompression lava pump (referring to Fig. 3) after atmospheric evaporation device temperature stabilization at 260 DEG C, Heat to decompression evaporator (adopting luwa evaporator), note observing decompression evaporator temperature change, when decompression evaporator temperature Reach more than 350 DEG C, just can open the valve between atmospheric evaporation device and decompression evaporator, about 5 minutes time, open decompression electricity Dynamic the oil good flow of Valve controlling, good flowmeter and valve switch, produced for the first time and opened with a small amount of, only valve opening door consumption 1/6th.
The oil that air-distillation goes out initially enters vacuum flasher and carries out vacuum flashing fractionation, and fractionation obtains constant-pressure and high-temperature Under oil ingredient and top oil gas, oil ingredient then enters decompression evaporator heating, and top oil gas is directly entered rectifying column, enters respectively Row scrapes Membrane Materials and oil gas enters tower fractionation.
Due to being in high vacuum state in decompression evaporator, going up oil mass for the first time, excessive to occur that evaporation produces not in time excessive Residual oil, and scraper plate is less with inwall gap, is preferably changed according to temperature change and vacuum system, electric current meets change, using by Gradually increase upper oil mass it is ensured that decompression evaporator load and condition of high vacuum degree, to ensure oil quality, now note observing decompression Residual oil amount in evaporator temperature, and decompression evaporator, decompression evaporator temperature should be at 350 DEG C -372 DEG C, residual oil journey rice-shaped.
Oil gas in decompression evaporator is constantly scraped Membrane Materials with knifing machine and is ascended into rectifying column.Now rectifier bottoms temperature Degree is in be gradually increasing trend.
(6) rectifying
After oil gas enters rectifying column, rectifier bottoms temperature is in be gradually increasing trend.Temperature in rectifying column is from bottom to top It is divided into four sections.Referring to Fig. 2.
1. bottom temp reached 300 DEG C of gas phase temperature in 20 minutes, and robot control system(RCS) table display bottom temp is 280-310 ℃.
2. one section of temperature can rise with the continuous gathering of bottom oil gas and physical change, and one section of temperature is filled in oil gas 280-290 DEG C is reached, now in one section of rectifying column, a part can be coagulated the oil getting off and enter and subtracted three line connects by backflow in the case of being full of In closed cans.
3. two sections of temperature, rises with one section of temperature and reaches 240-260 DEG C, and two sections of temperature are reflux temperature in a section.
4. three sections of temperature, the control of three sections of temperature is more crucial, should be when three sections of oil gas of rectifying column fill to 220 DEG C Open in robot control system(RCS) and subtract third fractional oil reflux pump, using the effect of condenser, full oil gas is carried out returned cold and congeal into the line that subtracts three Oil, after backflow is opened pump reflux with one section in flow back and act on simultaneously, output maximum ratio subtract third fractional oil, three sections of temperature are normal It is maintained at 150-185 DEG C, the yield ratio of the line that subtracts three is 60%.
5. four sections of temperature, the change of this section of temperature affects the quality of second line of distillation oil and first vacuum side stream, four sections of temperature Control more crucial, four sections of temperature should be between 120-150 DEG C.Because four sections of temperature are tower top temperature, as too high in temperature can produce Diesel component, in addition vacuum can because in tower temperature too high and be affected, load and the shadow of whole rectifying column can be increased The sound line that subtracts three, the output and quality of second line of distillation oil.
After each section of temperature of rectifying column is normal, three line reflux pumps and two wires reflux pump pass through self-con-tained unit according to technological requirement Voluntarily work, the produced quantity ratio subtracting third fractional oil controls 60%, color is in blackish green, and temperature is 245 DEG C, i.e. base oil main product Product 250sn;Second line of distillation oil produced quantity is 15%, i.e. base oil 150sn;First vacuum side stream produced quantity 7%, i.e. base oil 75sn.Subtract Pressure residual oil amount is 15%.
In rectifying column the overhead oil of output, third fractional oil and two wires oil not by overhead oil receive tank, third fractional oil receive tank and Two wires oil receives tank and receives.Overhead oil receives after tank receives overhead oil and is stored in overhead oil holding vessel.
The oil that rectifying column fractionates out, when 120 DEG C -150 DEG C, by the mass ratio of oil and carclazyte 5:0.6~5:1, adds in oil Enter carclazyte, circulated 15 minutes -45 minutes by stripper, remove the peculiar smell that distillation produces.
(7) solvent refining:
Product purification, the refined of readymade oil mainly carries out steam extracting with stripper, that is, utilize steam generator output Steam, the impurity contained by double product oil in corresponding treatment tank, colloidal bitumen and smell are rinsed, and overheated steaming used by stripping Steam flow amount unity loop control.Stripper is also under a reduced pressure, quantity of steam therefore to be controlled, and oily liquid in treatment tank Position, in order to avoid cause to rush tower phenomenon.
When refined hand-dipping liquid level is in refined tankage size 65%-75%, nmp (n- methylpyrrole can be carried out Alkanone) solvent extraction refine, add oil mass quality 10%-40% nmp (n- methyl pyrrolidone) carry out solvent refining.Due to It is vacuum state in treatment tank, therefore solvent enters treatment tank using from pumping mode formula, because solvent is taken in oil product mixed process Carry a certain amount of air, easily cause oxidation under the high temperature conditions, colorimetric is gone up, affect product quality.In order to avoid this phenomenon Generation, take and first the oil in treatment tank be cooled to 100 DEG C -120 DEG C, referring to Fig. 4.It is then turned on agitator, carry out solvent Extracting absorption.
Third fractional oil after refined and two wires oil are stored in finished pot after filter filtration.
Above-mentioned technique is all completed it is achieved that producing and processing automation, safety by dcs control system (Distributed Control System) Change, standardize.
Dcs control system has breakthrough in waste lubricant oil regeneration industry, for ensureing equipment safety, steady, long week Phase, run with high-quality at full capacity, improve the reliability that automatically controls it is ensured that production safety, this device adopts dcs to control system System, carries out centralized Control, monitoring, record and reports to the police to full device technical process.Dcs show comprehensively, directly perceived, accurately, controlling can Lean on, easy to operate it is achieved that computer digital animation, each parameter accurately shows.
In lubricating oil regeneration process, major embodiment is in the following areas:
(1) control to decompression evaporator and vacuum rectification tower vacuum and monitoring, warning system
(2) flow controls, and electrically operated valve is started and closes down, and the monitoring of uninterrupted
(3) Liquid level to each segmentation Atmospheric vacuum and monitoring, bound, early warning system heating system, frequency conversion system Control monitoring.
(4) temperature control to each section, reference record, control and warning exigency stop system.

Claims (5)

1. a kind of refining process of producing base oil by regenerating waste lubricating oil, including abjection solid waste, solvent pre-treatment, flocculation treatment, Air-distillation, vacuum distillation, rectifying and solvent refining, is characterized in that:
(1) deviate from solid waste:
Centrifugation removes the solid waste in the waste lubricating oil collected;
(2) solvent pre-treatment:
No. 120 solvent naphthas and the methyl tertiary butyl ether(MTBE) ratio of 1:1~1:5 in mass ratio are mixed, makes mixed solvent, will Waste lubricating oil and the mixed solvent ratio of 1:1.5~1:2 in mass ratio are mixed, stirring, standing, isolate poly-doped impurity and Moisture;Take upper strata oil, after removing the solvent in the oil of upper strata, obtain feedstock oil;
(3) flocculation treatment:
In feedstock oil, the ratio of 1:0.5~1:1 injects flocculant, 1:0.01 in mass ratio in feedstock oil simultaneously in mass ratio The ratio of~1:0.05 adds sodium hydroxide solution or potassium hydroxide solution, stirs 0.5 hour -2 hours, becomes flocculation mixing Thing;
(4) air-distillation:
Flocculated mixture, in 110 DEG C of -150 DEG C of the pre-heat treatment, obtains top light oil gas and bottom heavy constituent;Top light oil gas enters Atmospheric flash tower carries out Oil-gas Separation, and as fuel after the gas isolated is condensed, the light oil distributing recycles;Under Portion's heavy constituent entrance atmospheric evaporation device is heated to 260 DEG C -340 DEG C and carries out air-distillation;
(5) vacuum distillation:
The oil that air-distillation goes out carries out vacuum flashing fractionation first, obtains top oil gas and bottom oil ingredient, top oil gas It is directly entered rectifying column fractionation, oil ingredient enters decompression evaporator and carries out scraping Membrane Materials, and the oil gas that knifing distills out constantly rises Enter rectifying column;
(6) rectifying:
The oil gas that vacuum distillation goes out enters rectifying column, separates residual oil;The oil that rectifying column fractionates out when 120 DEG C -150 DEG C, by oil With the mass ratio of carclazyte 5:0.6~5:1, oil adds carclazyte, is circulated 15 minutes -45 minutes by stripper, remove distillation The peculiar smell producing;
(7) solvent refining:
In rectifying column, the oil of output enters in treatment tank, when refined hand-dipping liquid level is in refined tankage size 65%-75% When, add the n- methyl pyrrolidone of oil mass quality 10%-40% to carry out solvent refining.
2. the refining process of producing base oil by regenerating waste lubricating oil according to claim 1, is characterized in that, in described step (3) Sodium hydroxide solution or potassium hydroxide solution press NaOH or potassium hydroxide with water quality the proportions than 1:4~5:8.
3. the refining process of producing base oil by regenerating waste lubricating oil according to claim 1, is characterized in that, in described step (4) Oil-gas Separation is to carry out when atmospheric flash tower internal upper part temperature is 160 DEG C to 220 DEG C.
4. the refining process of producing base oil by regenerating waste lubricating oil according to claim 1, is characterized in that, in described step (4) In described atmospheric evaporation device, the Liquid level of heavy constituent is the 30%~70% of atmospheric evaporation device capacity.
5. the refining process of producing base oil by regenerating waste lubricating oil according to claim 1, is characterized in that, in described step (7) Solvent refining is first the oil in treatment tank to be cooled to 100 DEG C -120 DEG C, then stirs, and carries out solvent extraction absorption.
CN201610749463.7A 2016-08-29 2016-08-29 Refining technique of base oil regenerated from used lubrication oil Pending CN106336939A (en)

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CN106883925A (en) * 2017-04-28 2017-06-23 台州市绿保物资回收有限公司 A kind of waste lubricating oil refines regeneration method
CN106905991A (en) * 2017-04-18 2017-06-30 徐思玉 Black used oil is evaporated in vacuo system and process
CN107400556A (en) * 2017-09-05 2017-11-28 江苏川钿电气机械有限公司 The renovation process of waste lubricating oil
CN107513458A (en) * 2017-09-05 2017-12-26 江苏川钿电气机械有限公司 The refined renovation process of waste lubricating oil
CN107574012A (en) * 2017-10-16 2018-01-12 河北金谷再生资源开发有限公司 A kind of preparation method of producing base oil by regenerating waste lubricating oil
CN107880998A (en) * 2017-11-07 2018-04-06 盘锦阳光节能环保科技有限公司 A kind of Processes and apparatus of used oil recycling
CN108192716A (en) * 2018-02-27 2018-06-22 浙江绿保再生资源科技有限公司 A kind of waste lubricant oil regeneration all-in-one machine
CN108998083A (en) * 2018-08-14 2018-12-14 华侨大学 A kind of waste diesel regeneration method
CN109797037A (en) * 2019-01-11 2019-05-24 张长茂 A kind of distillation for processing of continous way waste lubricating oil
CN110093185A (en) * 2018-01-31 2019-08-06 王延海 Waste mineral oil Reclaimed Base Oil multiple-stage solvent extracts process for refining
CN110484345A (en) * 2019-07-29 2019-11-22 四川绿艺华福石化科技有限公司 A kind of method for regenerating waste lubricating oil
CN111068378A (en) * 2019-12-17 2020-04-28 湖州一环环保科技有限公司 Lubricating oil recovery processing device with pipeline edulcoration function
CN112159705A (en) * 2020-09-29 2021-01-01 甘肃环馨新能源科技有限公司 Waste mineral oil regeneration production process
CN114874836A (en) * 2022-05-16 2022-08-09 武汉工程大学 Waste lubricating oil regeneration process and system based on alkoxy carbon cation liquid

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CN106905991A (en) * 2017-04-18 2017-06-30 徐思玉 Black used oil is evaporated in vacuo system and process
CN106883925B (en) * 2017-04-28 2020-05-19 浙江绿保再生资源科技有限公司 Method for refining and regenerating waste lubricating oil
CN106883925A (en) * 2017-04-28 2017-06-23 台州市绿保物资回收有限公司 A kind of waste lubricating oil refines regeneration method
CN107400556A (en) * 2017-09-05 2017-11-28 江苏川钿电气机械有限公司 The renovation process of waste lubricating oil
CN107513458A (en) * 2017-09-05 2017-12-26 江苏川钿电气机械有限公司 The refined renovation process of waste lubricating oil
CN107574012A (en) * 2017-10-16 2018-01-12 河北金谷再生资源开发有限公司 A kind of preparation method of producing base oil by regenerating waste lubricating oil
CN107880998A (en) * 2017-11-07 2018-04-06 盘锦阳光节能环保科技有限公司 A kind of Processes and apparatus of used oil recycling
CN110093185A (en) * 2018-01-31 2019-08-06 王延海 Waste mineral oil Reclaimed Base Oil multiple-stage solvent extracts process for refining
CN108192716A (en) * 2018-02-27 2018-06-22 浙江绿保再生资源科技有限公司 A kind of waste lubricant oil regeneration all-in-one machine
CN108998083A (en) * 2018-08-14 2018-12-14 华侨大学 A kind of waste diesel regeneration method
CN109797037A (en) * 2019-01-11 2019-05-24 张长茂 A kind of distillation for processing of continous way waste lubricating oil
CN109797037B (en) * 2019-01-11 2022-05-03 张长茂 Continuous distillation treatment method for waste lubricating oil
CN110484345A (en) * 2019-07-29 2019-11-22 四川绿艺华福石化科技有限公司 A kind of method for regenerating waste lubricating oil
CN111068378A (en) * 2019-12-17 2020-04-28 湖州一环环保科技有限公司 Lubricating oil recovery processing device with pipeline edulcoration function
CN112159705A (en) * 2020-09-29 2021-01-01 甘肃环馨新能源科技有限公司 Waste mineral oil regeneration production process
CN114874836A (en) * 2022-05-16 2022-08-09 武汉工程大学 Waste lubricating oil regeneration process and system based on alkoxy carbon cation liquid
CN114874836B (en) * 2022-05-16 2023-03-14 武汉工程大学 Waste lubricating oil regeneration process and system based on alkoxy carbon cationic liquid

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