CN109868180A - A kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection - Google Patents
A kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection Download PDFInfo
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- CN109868180A CN109868180A CN201910327996.XA CN201910327996A CN109868180A CN 109868180 A CN109868180 A CN 109868180A CN 201910327996 A CN201910327996 A CN 201910327996A CN 109868180 A CN109868180 A CN 109868180A
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Abstract
The invention proposes a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection, process includes dehydrating and removing impurities, metallic sodium processing, faces hydrogen heat treatment, distillation unit.Waste lubricating oil enters atmospheric flash tower dehydration and de- light oil after filtering, waste lubricating oil after dehydrating and removing impurities is reacted with metal sodium powder at a certain temperature, unreacted metallic sodium enters after being reacted with the compound containing reactive hydrogen and faces hydrogen annealing device, subsequently into distilling in the thin film evaporator of thtee-stage shiplock, the fraction steamed is superior in quality base oil.The high chemical activity of this technology utilization metallic sodium, chlorohydrocarbon, additive and its decomposition product in waste lubricating oil, hydrocarbon oxidation product etc. can highly desirable be removed, Reclaimed Base Oil chlorinity and tenor are lower than 2mg/kg, carbon residue is down to 0.05% hereinafter, providing quality raw materials for follow-up hydrogenation purification.
Description
Technical field
The invention belongs to solid waste, environmental protection, petrochemical industries, are related to a kind of waste lubricating oil cyclic regeneration of environmental protection
Pretreating process.
Background technique
Domestic and international waste lubricant oil regeneration technology is developed so far, and is mainly had all through the ages sour technique, acidless craft and hydrogenation technique three
A stage.All it is towards few with worsening natural environment, waste lubricant oil regeneration technology in face of petering out for petroleum resources
Pollution, pollution-free direction are developed.
CN107574011A discloses a kind of complexing-membrane separation-hydrogenation-fractionation regeneration treating method of waste lubricating oil,
Include the following steps, complexing processing: waste lubricating oil and complexing agent aqueous solution are complexed；UF membrane: the mixture after complexing exists
Membrane separator carries out UF membrane, and raffinate is used as pitch blending stock after film, and clear liquid enters fixed bed hydrogenation and refines after film；Add hydrogen smart
System: clear liquid carries out hydrofinishing under the action of loaded catalyst after film, and the gas that hydrofinishing generates enters pipe network conduct
Fuel, liquid product enter atmospheric fractional tower；Normal pressure fractionation: the liquid product that hydrofinishing generates enters atmospheric fractional tower, often
Pressure fractionating top of tower is naphtha product, and atmospheric fractional tower side line is diesel product, and atmospheric fractional tower bottom is high-quality lubricating oil
Base oil.
CN107574012A discloses a kind of preparation method of producing base oil by regenerating waste lubricating oil, including pre-process,
The method that flash liberation, thin-film distillation, solvent extraction, solvent separated with base oil, were centrifuged decolorizing and refining produces base oil, wherein
Membrane-distillation distills mode using continuous multi-stage；Semi-finished product after distillation enter Multistage tower-type extraction equipment, with extractant carbonic acid
Dimethyl ester is sufficiently mixed uniformly by static plus dynamic gaseous mixture, repeatedly after multitple extraction, then is entering solvent recovering system time
Extra solvent is received, qualified base oil product is finally separated out by disk plate centrifuge.
Currently, the processing of China's waste lubricating oil is in the update stage, traditional soda acid technique is no longer satisfied
The requirement of China's processing and environmental protection of waste lubricating oil now, new technology and new process gradually replace traditional processing mode,
Hydrofining technology is process for regeneration of waste lubricating oil most with prospects.Solvent extraction, molecular distillation technique, membrane separation technique
It is moving to maturity Deng pretreatment new technology and is reaching the industrialized production stage, since the source of waste lubricating oil is complicated, respectively
Very greatly, these technologies expose that solvent consumption is big, solvent extraction interface is fuzzy, film is stifled to the variation of physical and chemical indexes in the industrial production
The problems such as plug, corrosive pipeline, column plate coking, heat exchanger blocking, has seriously affected safety and the length week of regenerator for waste lubricating oil
Phase operation.Pretreatment-hydrogenation technique be the waste lubricating oil fraction after pretreatment is made by hydrofinishing chlorine in oil product,
The objectionable impurities such as sulphur, oxygen, nitrogen be changed into corresponding hydrogen chloride, hydrogen sulfide, water, ammonia and remove, and make alkene and diene hydrogenation
Saturation, aromatic moiety add hydrogen to be saturated, to improve the quality of oil product.Base oil after hydrofinishing can achieve II class basis
The standard of oil, value of the product obtain maximum lift.Exploiting economy close friend, environment friendly and pollution-free pretreating process, effectively destroy
Additive in waste lubricating oil removes chlorohydrocarbon, metallorganic, colloid, asphalitine in waste lubricating oil, improves pretreatment dress
Anticorrosive, anti-coking the ability with hydrogenation plant is set, problem of environmental pollution and long period in Spent lube reclamation process are solved
Operation problem is the developing direction that waste lubricating oil in future recycles.
Summary of the invention
The purpose of the present invention is to provide a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection, solve existing useless
Corrosive pipeline that lubricant oil regeneration enterprise faces, column plate coking, secondary pollution is serious, recovery efficiency is low, is difficult to continuous-stable height
The problem of production, provides good raw material for follow-up hydrogenation purification.
To achieve the goals above, the technical solution adopted by the present invention includes dehydrating and removing impurities, metallic sodium processing, faces at hydrogen heat
Reason, distilation steps:
(1) dehydrating and removing impurities: with water vigorous reaction can occur for metallic sodium, generate hydrogen and sodium hydroxide, can also send out with solid impurity
Raw reaction, therefore in order to reduce the dosage of metallic sodium and guarantee the safe operation of device, waste lubricating oil first must thoroughly remove water
Divide and filter, becomes clean dry waste oil.Waste lubricating oil exchanges heat through heat exchanger to 180 after filter device removes solid impurity
DEG C or more enter atmospheric flash tower be dehydrated and extract light oil, tower bottom oil is clean dry waste oil；
(2) metallic sodium is handled: using the chemical reaction ability that metal sodium powder is very active, with the various polar objecies in waste lubricating oil
Various products of metamorphism reaction in miscellaneous element, waste oil in matter, organic molecule, is converted into the glue of sodium organic compound and condensation
Matter.It is injected into the reactor with stirring, is then sprayed into containing 0.2% ~ 4wt%'s after dry waste oil is exchanged heat to certain temperature
The slurries of finely divided metallic sodium are reacted, to remove unreacted after reacting a period of time with the compound containing reactive hydrogen
Metallic sodium.The operating condition of metallic sodium processing are as follows: temperature is 130 ~ 230 DEG C, and the processing time is 60 ~ 110min；
(3) face hydrogen heat treatment: metallic sodium treated waste lubricating oil enters after heating furnace is warming up to certain temperature and faces at hydrogen heat
Reactor is managed, the operating condition of hydrogen heat treatment reactor is faced are as follows: temperature is 260 ~ 380 DEG C, and the processing time is 15 ~ 150min, pressure
Power is 0-0.9MPa；
Distill: face hydrogen heat treatment after waste lubricating oil after exchanging heat into thtee-stage shiplock thin film evaporator in distill, film
The operating condition of evaporator is: evaporating temperature is 160 ~ 320 DEG C, and absolute pressure is 10 ~ 120Pa, and what is obtained is good add
Hydrogen refined material.
The condition of the step (1) atmospheric flashing is preferred are as follows: atmospheric flash tower inlet temperature is 190 ~ 240 DEG C.
The River Bank Stability method of the step (2) finely divided metallic sodium is as follows: by two parts of technical white oils (40 DEG C of viscosity
10~24mm2/ s) 110 DEG C are heated to, a metal sodium powder is added with vigorous stirring, makes molten metal sodium with droplet
State is dispersed in white oil, becomes dispersion slurries, and average particle size is 30 μm.
Step (2) described in metallic sodium slurries dosage it is related with the quality good or not of waste lubricating oil, dosage is preferably waste oil
0.5% ~ 1.8 wt %.
Step (2) described in metallic sodium processing operating condition it is preferred are as follows: temperature be 130 ~ 200 DEG C, processing the time be 60
~90min。
Step (2) described in remove unreacted metallic sodium, available reactive hydrogen chemical combination with the compound containing reactive hydrogen
Object includes water, vapor, hydrogen peroxide, preferably water, and water consumption is 0.1% ~ 0.8 wt % of waste oil.
Step (3) described in face hydrogen heat treatment reactor operating condition are as follows: temperature be 290 ~ 380 DEG C, processing the time be
80 ~ 150min, pressure 0-0.9MPa.
Step (4) described in thtee-stage shiplock thin film evaporator, absolute pressure be 10 ~ 110Pa, temperature is respectively: level-one
Temperature is 160 ~ 210 DEG C, and second level temperature is 210 ~ 270 DEG C, and three-level temperature is 270 ~ 310 DEG C.
It is pre- with existing waste lubricating oil the present invention provides a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection
Processing technique is compared, it is advantageous that:
(1) the very active chemical reaction ability of metal sodium powder can highly desirable remove the chlorohydrocarbon in waste lubricating oil, add
Agent and its decomposition product, hydrocarbon oxidation product etc., can also react with solid impurity, and dechlorination and demetalization ratio are more thoroughly；
(2) the additive that hydrogen heat treatment further destroys in waste lubricating oil is faced, and ash-forming material is largely converted into and can be filtered to remove
Solid residue；
(3) a kind of non-equilibrium distillation that thin film evaporator carries out in high vacuum conditions, can be effectively removed in waste lubricating oil
Component is deteriorated, tenor, carbon residue and the ideal lubricant base oil fraction of the low-down quality of ash content are obtained.
Detailed description of the invention
Fig. 1 is technological process block-diagram of the invention；
A raw material, b filter device, c flash-evaporation dehydration take off light oil in figure, d metallic sodium is handled, e faces hydrogen heat treatment, f three-level film steams
Hair, g lube cut
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.
Embodiment 1: as shown in Figure 1, waste lubricating oil exchanges heat through heat exchanger to 190 after filter device removes solid impurity
DEG C enter atmospheric flash tower be dehydrated and extract light oil, tower bottom oil is clean dry waste oil；Dry waste oil is exchanged heat to infusing after 200 DEG C
Enter to stirring reactor in, then by the weight ratio of 1.1 wt %(and waste lubricating oil) finely divided metallic sodium slurries
Be injected in sodium treatment reactor, react 60min after, with the weight ratio of 0.6 wt %(and waste lubricating oil) water remove unreacted
Metallic sodium；Metallic sodium treated waste lubricating oil enters after heating furnace is warming up to 290 DEG C faces hydrogen heat treatment reactor,
130 min are handled under conditions of 290 DEG C；Waste lubricating oil after heat treatment enter heat exchanger heat exchange to after certain temperature successively into
Enter thin film evaporator, when carrying out thin film evaporation, pressure is set as 110Pa, and 210 DEG C of level-one temperature, 250 DEG C of second level temperature, three
310 DEG C of temperature of grade；Obtained base oil fractions enter subsequent hydrogenation plant and carry out hydrofinishing.
Embodiment 2: as shown in Figure 1, waste lubricating oil exchanges heat through heat exchanger to 210 after filter device removes solid impurity
DEG C enter atmospheric flash tower be dehydrated and extract light oil, tower bottom oil is clean dry waste oil；Dry waste oil is exchanged heat to infusing after 130 DEG C
Enter to stirring reactor in, then by the weight ratio of 1.8 wt %(and waste lubricating oil) finely divided metallic sodium slurries
Be injected in sodium treatment reactor, react 90min after, with the weight ratio of 0.8 wt %(and waste lubricating oil) water remove unreacted
Metallic sodium；Metallic sodium treated waste lubricating oil enters after heating furnace is warming up to 380 DEG C faces hydrogen heat treatment reactor,
80 min are handled under conditions of 380 DEG C；Waste lubricating oil after heat treatment enter heat exchanger heat exchange to after certain temperature successively into
Enter thin film evaporator, when carrying out thin film evaporation, pressure is set as 70Pa, and 200 DEG C of level-one temperature, 270 DEG C of second level temperature, three-level
300 DEG C of temperature；Obtained base oil fractions enter subsequent hydrogenation plant and carry out hydrofinishing.
Embodiment 3: as shown in Figure 1, waste lubricating oil exchanges heat through heat exchanger to 240 after filter device removes solid impurity
DEG C enter atmospheric flash tower be dehydrated and extract light oil, tower bottom oil is clean dry waste oil；Dry waste oil is exchanged heat to infusing after 160 DEG C
Enter to stirring reactor in, then by the weight ratio of 0.7 wt %(and waste lubricating oil) finely divided metallic sodium slurries
Be injected in sodium treatment reactor, react 80min after, with the weight ratio of 0.3 wt %(and waste lubricating oil) water remove unreacted
Metallic sodium；Metallic sodium treated waste lubricating oil enters after heating furnace is warming up to 360 DEG C faces hydrogen heat treatment reactor,
95 min are handled under conditions of 360 DEG C；Waste lubricating oil after heat treatment enter heat exchanger heat exchange to after certain temperature successively into
Enter thin film evaporator, when carrying out thin film evaporation, pressure is set as 10Pa, and 160 DEG C of level-one temperature, 210 DEG C of second level temperature, three-level
270 DEG C of temperature；Obtained base oil fractions enter subsequent hydrogenation plant and carry out hydrofinishing.
Embodiment 4: as shown in Figure 1, waste lubricating oil exchanges heat through heat exchanger to 230 after filter device removes solid impurity
DEG C enter atmospheric flash tower be dehydrated and extract light oil, tower bottom oil is clean dry waste oil；Dry waste oil is exchanged heat to infusing after 180 DEG C
Enter to stirring reactor in, then by the weight ratio of 0.5 wt %(and waste lubricating oil) finely divided metallic sodium slurries
Be injected in sodium treatment reactor, react 70min after, with the weight ratio of 0.1 wt %(and waste lubricating oil) water remove unreacted
Metallic sodium；Metallic sodium treated waste lubricating oil enters after heating furnace is warming up to 340 DEG C faces hydrogen heat treatment reactor,
150 min are handled under conditions of 340 DEG C；Waste lubricating oil after heat treatment enter heat exchanger heat exchange to after certain temperature successively into
Enter thin film evaporator, when carrying out thin film evaporation, pressure is set as 50Pa, and 180 DEG C of level-one temperature, 240 DEG C of second level temperature, three-level
300 DEG C of temperature；Obtained base oil fractions enter subsequent hydrogenation plant and carry out hydrofinishing.
Crude lube stock and its base oil fractions property in 1 embodiment of table
Claims (9)
1. a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection, which is characterized in that at dehydrating and removing impurities, metallic sodium
The process of hydrogen heat treatment, distillation is managed, faces, specifically includes the following steps:
(1) dehydrating and removing impurities: with water vigorous reaction can occur for metallic sodium, generate hydrogen and sodium hydroxide, can also send out with solid impurity
Raw reaction, therefore in order to reduce the dosage of metallic sodium and guarantee the safe operation of device, waste lubricating oil first must thoroughly remove water
Divide and filter, become clean dry waste oil, waste lubricating oil exchanges heat through heat exchanger to 180 after filter device removes solid impurity
DEG C or more enter atmospheric flash tower be dehydrated and extract light oil, tower bottom oil is clean dry waste oil；
(2) metallic sodium is handled: using the chemical reaction ability that metal sodium powder is very active, with the various polar objecies in waste lubricating oil
Various products of metamorphism reaction in miscellaneous element, waste oil in matter, organic molecule, is converted into the glue of sodium organic compound and condensation
Matter is injected into the reactor with stirring after dry waste oil exchanges heat to certain temperature, is then sprayed into containing 0.2% ~ 4wt%'s
The slurries of finely divided metallic sodium are reacted, to remove unreacted after reacting a period of time with the compound containing reactive hydrogen
Metallic sodium, metallic sodium processing operating condition are as follows: temperature be 130 ~ 230 DEG C, the processing time be 60 ~ 110min；
(3) face hydrogen heat treatment: metallic sodium treated waste lubricating oil enters after heating furnace is warming up to certain temperature and faces at hydrogen heat
Reactor is managed, the operating condition of hydrogen heat treatment reactor is faced are as follows: temperature is 260 ~ 380 DEG C, and the processing time is 15 ~ 150min, pressure
Power is 0-0.9MPa；
Distill: face hydrogen heat treatment after waste lubricating oil after exchanging heat into thtee-stage shiplock thin film evaporator in distill, film
The operating condition of evaporator is: evaporating temperature is 160 ~ 320 DEG C, and absolute pressure is 10 ~ 120Pa, and what is obtained is good add
Hydrogen refined material.
2. a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection according to right 1, which is characterized in that the step
The condition of the rapid (1) described atmospheric flashing are as follows: atmospheric flash tower inlet temperature is 190 ~ 240 DEG C.
3. a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection according to right 1, which is characterized in that the step
Suddenly (2) in finely divided metallic sodium River Bank Stability method it is as follows: by two parts of technical white oils (40 DEG C of 10 ~ 24mm of viscosity2/ s) heating
To 110 DEG C, a metal sodium powder is added with vigorous stirring, molten metal sodium is made to be dispersed in white oil with the state of droplet
In, become dispersion slurries, average particle size is 30 μm.
4. a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection according to right 1, which is characterized in that the step
Suddenly (2) the dosage of middle metallic sodium slurries is related with the quality good or not of waste lubricating oil, and dosage is preferably 0.5% ~ 1.8 wt % of waste oil.
5. a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection according to right 1, which is characterized in that the step
Suddenly (2) the operating condition of middle metallic sodium processing is preferred are as follows: temperature is 130 ~ 200 DEG C, and the processing time is 60 ~ 90min.
6. a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection according to right 1, which is characterized in that the step
Suddenly (2) in the compound containing reactive hydrogen remove unreacted metallic sodium, available active dydrogen compounds include water, vapor,
Hydrogen peroxide, preferably water, water consumption are 0.1% ~ 0.8 wt % of waste oil.
7. a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection according to right 1, which is characterized in that the step
Suddenly (3) in face the operating condition of hydrogen heat treatment reactor are as follows: temperature is 290 ~ 380 DEG C, and the processing time is 80 ~ 150min, and pressure is
0-0.9MPa。
8. a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection according to right 1, which is characterized in that the step
The thin film evaporator of rapid (4) middle thtee-stage shiplock, temperature is respectively: level-one temperature is 160 ~ 210 DEG C, and second level temperature is 210 ~ 270
DEG C, three-level temperature is 270 ~ 310 DEG C.
9. a kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection according to right 1, which is characterized in that the step
Suddenly (4) middle absolute pressure is 10 ~ 110Pa.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111876197A (en) * | 2020-07-28 | 2020-11-03 | 湖北润驰环保科技有限公司 | Pretreatment process for treating waste lubricating oil by chemical refining method |
| CN113117685A (en) * | 2021-04-21 | 2021-07-16 | 湖北润驰环保科技有限公司 | Waste lubricating oil de-ironing agent and preparation method thereof |
| CN114317094A (en) * | 2021-12-27 | 2022-04-12 | 江苏洋井环保服务有限公司 | Pollution-reducing continuous regeneration pretreatment device and process for waste engine oil |
| CN114437863A (en) * | 2022-02-21 | 2022-05-06 | 湖北安耐吉环保科技有限公司 | Regeneration pretreatment process for waste lubricating oil |
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Cited By (4)
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