CN102504933A - Regeneration method of waste lubricating oil - Google Patents
Regeneration method of waste lubricating oil Download PDFInfo
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- CN102504933A CN102504933A CN2011103650258A CN201110365025A CN102504933A CN 102504933 A CN102504933 A CN 102504933A CN 2011103650258 A CN2011103650258 A CN 2011103650258A CN 201110365025 A CN201110365025 A CN 201110365025A CN 102504933 A CN102504933 A CN 102504933A
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Abstract
The invention provides a regeneration method of waste lubricating oil which at least comprises the steps of waste oil pretreatment, short path distillation and hydrofining. Compared with the prior art, the invention has the advantages that the technology is simple, the operation is flexible, no pollution is caused, all the quality indexes of produced lube base oil meet the standard requirements of universal base oil of lubricating oil, and the produced lube base oil can be used for preparing various lubricating oil products. Therefore, the regeneration method of the waste lubricating oil has a wider application range and is more environment-friendly.
Description
Technical field
The present invention relates to a kind of renovation process of waste lubricating oil.
Background technology
Along with the further investigation and the development of process for regeneration of waste lubricating oil technology, the treatment capacity of the industrialized unit of waste lubricant oil regeneration is also increasing, and is therefore also increasingly high to environmental requirement." process engineering for regenerating of waste lubricating oil " (patent No.: ZL200610086926.2) few, simple to operate, the good product quality of clay treatment process facility investment of patent employing is the first-selected process for purification of middle-size and small-size waste lubricant oil regeneration device.When the treatment capacity of waste lubricant oil regeneration device increased, the quantity of the useless clay dregs of clay-filtered generation also increased thereupon, brought certain difficulty for the harmless treatment of useless clay dregs.Unifining is a kind of cleaning procedure, does not produce the oil-containing argil slag, and the quality of lube base oil prodn is good, yield also increases.The present invention is used for waste lubricant oil regeneration with autonomous improved hydrogen refining process and handles, and for building large-scale waste lubricant oil regeneration device the advanced technologies technology of clean environment firendly more is provided.
Handle in the practice at waste lubricant oil regeneration and to find, the waste lubricating oil raw material type of collection is many, form complicacy, some inferior raw material even influence the normal operation of subsequent technique.Therefore, improve, make this Technology wider the accommodation of raw material for pretreatment technology.
Summary of the invention
The objective of the invention is improve to improve and expansion " process for regeneration of waste lubricating oil technology " patent (patent No.: ZL200610086926.2), provide a kind of scope of application more extensively, the waste lubricant oil regeneration method of environmental protection more.
Above-mentioned purpose of the present invention realizes through following technical scheme:
A kind of waste lubricant oil regeneration method is provided, comprises waste oil pre-treatment, short-path distillation and unifining several steps at least, concrete steps are following:
(1) waste oil pre-treatment: with the mixing tank that waste lubricating oil places a band to stir, add the basic cpd of waste lubricating oil weight 0-5.0%, under room temperature to 100 ℃ condition, stirred 10-60 minute; Moved into the slurry tank sedimentation then 1-10 hour; The preferred basic cpd that adds waste lubricating oil weight 0.5～1.0% stirred 20～40 minutes down at 60～90 ℃, and sedimentation is 10 hours then; The basic cpd that most preferably adds waste lubricating oil weight 0.5-1.0%; Stirred 40 minutes down for 90 ℃ in temperature, sedimentation is 10 hours then, to remove moisture and impurity;
(2) short-path distillation: the waste oil that step (1) was handled gets into short-path distillation, and will pass through following two-step distillation successively at least: first step short-path distillation fractionates out the light lubricating oil oil base stock, and operational condition is temperature 150-250 ℃, vacuum tightness 30-100Pa; Preferred operational condition is: temperature 170-200 ℃, and vacuum tightness 30-50Pa; Then material get into second stage short-path distillation steam in the matter lube oil base stocks, Residual oil is discharged at the bottom of by tower, its operational condition is temperature 180-260 ℃, vacuum tightness 5-20Pa; The preferred operations condition is temperature 200-230 ℃, vacuum tightness 5-10Pa.
(3) unifining: the various lube oil base stocks that distill out through step (2) get into hydro-refining unit respectively; Under hydrogenation catalyst catalysis, react; Its main operational condition is: temperature 150-350 ℃, hydrogen dividing potential drop are 1.0-10.0MPa, hydrogen-oil ratio 10-200m
3/ m
3, air speed 1.0-5.0h
-1, the preferred operations condition is: temperature 150-180 ℃, hydrogen dividing potential drop 1.0-2.0MPa, hydrogen-oil ratio 30-50m
3/ m
3, air speed 1.5-2.5h
-1, remove trace impurity and decolouring in the oil product thus, produce the high quality lubricant base.
Method of the present invention preferably takes a step forward and comprises rectification step with short-path distillation after pre-treatment, is about to the pretreated waste oil of step (1) and gets into rectifying tower after filtering, its operational condition: temperature is that 130-200 ℃, vacuum tightness are 150-350Pa; Preferred operational condition is that temperature 150-170 ℃, vacuum tightness are 240-260Pa; Better remove water and/or the light Fuel that contains in the waste lubricating oil with this.
The described basic cpd of step (1) can be one or more the mixture in inorganic alkaline compound or the organic basic compound; The mixture of one or more in preferred sodium hydroxide, calcium hydroxide or alcamines or the ethyleneamines compounds; Any one in the ethyleneamines compounds or mix ethyleneamines most preferably.
The described short-path distillation of step (2) also preferably further comprises third stage short-path distillation; Be that the material behind the matter lube oil base stocks got into third stage short-distance distiller during said second stage short-path distillation steamed, its operational condition is temperature 200-300 ℃, vacuum tightness 4-7Pa; The preferred operations condition is temperature 230-250 ℃; Vacuum tightness 4-6Pa steams the heavy grease oil base stock, and Residual oil is discharged at the bottom of by tower.
Step (3) The hydrogenation catalyst may be selected from iron - cobalt-molybdenum catalyst or - molybdenum hydrotreating catalyst, other types of catalysts.
The present invention is a kind of combination process; Method is simple, be prone to row, and used equipment all is petroleum chemical industry equipment commonly used, domesticly all can make; And flexible operation; Can come the control manipulation condition according to performance, composition and the boiling range scope of waste oil, therefore be applicable to and handle various waste lubricating oils, and the beneficial effect with following several respects:
1. compared with prior art, waste lubricant oil regeneration method of the present invention has adopted hydrorefined step, and the characteristics of hydrogenation process are no clay dregs, can be applicable to large and medium-sized oil reclaimer; Can improve base oil yield 1%-10%.
2. all operations at a lower temperature of each technique unit of the present invention not oxidation in the course of processing, do not decompose, thereby purpose product lubricant base yield are high, generally can reach more than 80%.
In sum; The present invention compared with present technology, technology is simple, flexible operation; Pollution-free; The lubricant base quality index of producing all reaches the requirement of lubricating oil general basic oil standard, can be used for modulating various lube product, and therefore lubricant oil regeneration method of the present invention has bigger social benefit and economic benefit.
Embodiment
Further specify characteristics of the present invention through specific examples below.
Embodiment 1.
The used waste lubricating oil character of present embodiment is seen table 1.
The 10kg waste lubricating oil is passed through steps of processing:
(1) pre-treatment
Mixing tank with waste lubricating oil places a band to stir stirred 20 minutes under 60 ℃ of conditions, moved into the slurry tank sedimentation then 10 hours, removed moisture and mechanical impurity;
(2) rectifying:
The pretreated waste oil of step (1) is got into rectifying tower, its operational condition after filtering: temperature is that 150-170 ℃, vacuum tightness are 240-260Pa;
(3) short-path distillation
The waste oil that step (2) was handled gets into short-path distillation, and pass through following three-stage distillation successively: first step short-path distillation operational condition is temperature 170-200 ℃, vacuum tightness 30-50Pa, fractionates out the light lubricating oil oil base stock; Material gets into second stage short-path distillation then; Its operational condition is temperature 200-230 ℃, vacuum tightness 5-10Pa, matter lube oil base stocks in steaming, and material gets into third stage short-distance distiller then; Its operational condition is temperature 230-250 ℃; Vacuum tightness 4-6Pa steams the heavy grease oil base stock, and Residual oil is discharged at the bottom of by tower;
(4) unifining:
Through step (3) distill out light, in and the heavy grease oil base stock get into hydro-refining unit respectively, under iron-molybdenum catalyst catalysis, react, its main operating condition is: temperature 150-180 ℃, hydrogen dividing potential drop are 1.0-2.0MPa, hydrogen-oil ratio 30-50m
3/ m
3, air speed 1.5-2.5h
-1, remove trace impurity and decolouring in the oil product thus, obtain HVI100, HVI200 and three kinds of lube base oil products of HVI350, three kinds of product properties see Table 2.
Table 1 waste lubricating oil raw material properties
| Project | The waste lubricating oil raw material |
| Outward appearance | Black non transparent |
| Kinematic viscosity (40 ℃) mm 2/s | 87 |
| Proportion | 880.7 |
| Flash-point (opening), ℃ | 192 |
| Water, % | 0.10 |
| Mechanical impurity, % | 0.23 |
| Acid number, mgKOH/g | 1.16 |
| Carbon residue, % | 1.76 |
| Sulphur, μ g/g | 4040 |
| Nitrogen, μ g/g | 1692 |
| Colloid, % | 14.1 |
| Quantity of distillate before 370 ℃, % | 8.03 |
| Metal content, μ g/g | |
| Iron | 34.1 |
| Calcium | 930.8 |
| Zinc | 753.2 |
Table 2 lubricant base product property
Can find out that from table 2 data lubricant base HVI100, HVI200, three kinds of products of HVI350 have all reached China's all-purpose engine oil base oil standard.
(patent No.: ZL200610086926.2) compare, the lubricant base yield improves about 10% with " process engineering for regenerating of waste lubricating oil ".
Embodiment 2
The used waste lubricating oil character of present embodiment is seen table 3.
The 10kg waste lubricating oil is passed through steps of processing:
(1) pre-treatment:
With the mixing tank that waste lubricating oil places a band to stir, the nitrogen content that adds waste lubricating oil weight 0.5-1.0% by weight percentage is at 40～41% mixing ethyleneamines.Under 90 ℃ of conditions, stirred 40 minutes, moved into the slurry tank sedimentation then 10 hours, remove moisture and impurity.
(2) rectifying:
The pretreated waste oil of step (1) is got into rectifying tower, operational condition after filtering: temperature is 150-170 ℃, and vacuum tightness is 250-260Pa.
(3) short-path distillation:
The waste oil that step (2) was handled gets into short-path distillation, and pass through following three-stage distillation successively: first step short-path distillation operational condition is temperature 170-200 ℃, vacuum tightness 30-50Pa; Second stage short-path distillation operational condition is temperature 200-230 ℃, vacuum tightness 5-10Pa, and third stage short-path distillation operational condition is temperature 230-250 ℃, vacuum tightness is 4-6Pa.
(4) unifining:
The lubricant base that distills out through step (3) gets into hydro-refining unit respectively, and its operational condition is: temperature 150-180 ℃, and hydrogen dividing potential drop 1.0-2.0MPa; Hydrogen-oil ratio 30-50m
3/ m
3, air speed 1.5-2.5h
-1
Obtain HVI100 through (1)-(4) steps, HVI, 200 with three kinds of lube base oil prodns of HVI350, its character is seen table 4.
Table 3 waste lubricating oil feedstock property
| Project | The waste lubricating oil feedstock property | Remarks |
| Outward appearance | Greyish black muddiness, opaque | |
| Kinematic viscosity (40 ℃) mm 2/s | 58.06 | |
| Proportion | - | Water, uncertainty are arranged |
| Flash-point (opening), ℃ | - | Water, uncertainty are arranged |
| Water, % | ＞5 |
| Mechanical impurity, % | 0.57 | |
| Acid number, mgKOH/g | 1.87 | |
| Carbon residue, % | 1.37 | |
| Sulphur, μ g/g | 3762 | |
| Nitrogen, μ g/g | 1285 | |
| Colloid, % | 16.3 | |
| Quantity of distillate before 370 ℃, % | 17.2 | |
| Metal content, μ g/g | ||
| Iron | 96.3 | |
| Calcium | 907 | |
| Zinc | 493 |
Table 4 lubricant base quality product
Table 3 data declaration, waste lubricating oil raw water content is high, the greyish black muddiness of outward appearance, and acid number is high simultaneously, gum level is also high, explains that this waste oil deterioration by oxidation is serious, is a typical waste lubricating oil raw material inferior.
Can find out that from table 4 data through three kinds of lube base oil prodn HVI100 of present embodiment method processing treatment, HVI200 and HVI350 have all reached China's all-purpose engine oil base oil standard.
Because water-content and light Fuel component concentration are all higher in the waste lubricating oil raw material, the lubricating oil component actual content is lower in the waste oil, so the lubricant base yield of product is also low than embodiment 1.
Renovation process through embodiment 2 explanations waste lubricating oil provided by the invention can manipulation of regeneration waste lubricating oil raw material inferior.
Claims (10)
1. a waste lubricant oil regeneration method is characterized in that, comprises following step at least:
(1) waste oil pre-treatment: the mixing tank that waste lubricating oil is placed a band stirring; The basic cpd that adds waste lubricating oil weight 0-5.0%; Under room temperature to 100 ℃ condition, stirred 10-60 minute, moved into the slurry tank sedimentation then 1-10 hour, to remove moisture and impurity;
(2) short-path distillation: the waste oil that step (1) was handled gets into short-path distillation, and pass through following two-step distillation at least successively: first step short-path distillation operational condition is temperature 150-250 ℃, vacuum tightness 30-100Pa, fractionates out the light lubricating oil oil base stock; Material gets into second stage short-path distillation then, and its operational condition is temperature 180-260 ℃, vacuum tightness 5-20Pa, and matter lube oil base stocks in steaming, Residual oil are discharged at the bottom of by tower;
(3) unifining: the various lube oil base stocks that distill out through step (2) get into hydro-refining unit respectively; Under hydrogenation catalyst catalysis, react; Its main operational condition is: temperature 150-350 ℃, hydrogen dividing potential drop are 1.0-10.0MPa, hydrogen-oil ratio 10-200m
3/ m
3, air speed 1.0-5.0h
-1, remove trace impurity and decolouring in the oil product thus, produce the high quality lubricant base.
2. the described waste lubricant oil regeneration method of claim 1; It is characterized in that: after pre-treatment, take a step forward and comprise rectification step with short-path distillation; Be about to the pretreated waste oil of step (1) and get into rectifying tower after filtering; Its operational condition: temperature is that 130-200 ℃, vacuum tightness are 150-350Pa, to remove water and/or the light Fuel that contains in the waste lubricating oil.
3. the described waste lubricant oil regeneration method of claim 2 is characterized in that: said rectifying tower operational condition is that temperature 150-170 ℃, vacuum tightness are 240-260Pa.
4. the described waste lubricant oil regeneration method of claim 1 is characterized in that: the described basic cpd of step (1) is selected from one or more the mixture in sodium hydroxide, calcium hydroxide, alcamines or the ethyleneamines compounds.
5. the described waste lubricant oil regeneration method of claim 1, it is characterized in that: the described pretreated operational condition of step (1) is: add the basic cpd of waste lubricating oil weight 0.5-1.0%, stirred 40 minutes down for 90 ℃ in temperature, sedimentation is 10 hours then.
6. the described waste lubricant oil regeneration method of claim 1, it is characterized in that: the operational condition of the described short-path distillation of step (2) is: 170-200 ℃ of first step short-path distillation service temperature, vacuum tightness 30-50Pa; Second stage short-path distillation service temperature is 200-230 ℃, vacuum tightness 5-10Pa.
7. the described waste lubricant oil regeneration method of claim 1; It is characterized in that: in the short-path distillation of step (2), further comprise third stage short-path distillation; Be that the material behind the matter lube oil base stocks got into third stage short-distance distiller during said second stage short-path distillation steamed, its operational condition is temperature 200-300 ℃, vacuum tightness 4-7Pa; Steam the heavy grease oil base stock, Residual oil is discharged at the bottom of by tower.
8. the described waste lubricant oil regeneration method of claim 7, it is characterized in that: said third stage short-distance distiller operational condition is: temperature 230-250 ℃, vacuum tightness 4-6Pa.
According to claim 1, wherein the waste oil regeneration method characterized in that: in step (3) of the hydrotreating catalyst is selected from iron - cobalt-molybdenum catalyst or - molybdenum catalyst.
10. the described waste lubricant oil regeneration method of claim 1, it is characterized in that: the described hydrorefined operational condition of step (3) is: temperature 150-180 ℃, hydrogen dividing potential drop 1.0-2.0MPa, hydrogen-oil ratio 30-50m
3/ m
3, air speed 1.5-2.5h
-1
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045298A (en) * | 2012-12-27 | 2013-04-17 | 宜昌升华新能源科技有限公司 | System for recovering cracking fraction fuel in waste oil |
| CN103351939A (en) * | 2013-06-28 | 2013-10-16 | 姜皓 | Refine and regeneration method of waste lubricant oil and regeneration device thereof |
| CN104178210A (en) * | 2013-05-27 | 2014-12-03 | 山东恒导石油化工股份有限公司 | Method and technological apparatus for recovering waste high-boiling-point heat-transfer oil |
| CN104531324A (en) * | 2014-11-28 | 2015-04-22 | 刘林 | Method for producing gear lubricating oil by using recovered lubricating oil |
| CN104560354A (en) * | 2014-12-24 | 2015-04-29 | 惠州Tcl环境科技有限公司 | Method and system for recycling and regenerating waste mineral oil |
| CN105001968A (en) * | 2015-06-30 | 2015-10-28 | 廖莱 | Technology for refining light and heavy lubricant base oil from waste engine oil |
| CN106147857A (en) * | 2016-08-19 | 2016-11-23 | 董琳 | A kind of environmentally friendly internal combustion engine used oil recycling technique |
| CN106693433A (en) * | 2017-02-04 | 2017-05-24 | 深圳市三环再生科技有限公司 | Waste lubricating oil regeneration distillation additive and application method thereof |
| CN107254329A (en) * | 2017-07-12 | 2017-10-17 | 宁波中循环保科技有限公司 | waste lubricating oil processing method |
| CN107353996A (en) * | 2017-07-31 | 2017-11-17 | 奇台县佳浩工程建设有限公司 | Waste lubricant oil regeneration utilization process and its process units |
| CN108998091A (en) * | 2018-09-12 | 2018-12-14 | 山东齐创石化工程有限公司 | Waste mineral oil regeneration technique |
| CN109233988A (en) * | 2018-08-06 | 2019-01-18 | 天津大学 | The clean high-valued recycling and reusing method and apparatus of waste lubricating oil |
| CN118594531A (en) * | 2024-05-30 | 2024-09-06 | 重庆工商大学 | Waste wind power lubricating oil hydrogenation catalyst, preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103045298A (en) * | 2012-12-27 | 2013-04-17 | 宜昌升华新能源科技有限公司 | System for recovering cracking fraction fuel in waste oil |
| CN103045298B (en) * | 2012-12-27 | 2016-03-16 | 宜昌升华新能源科技有限公司 | A kind of system reclaiming cracking cut fuel oil for waste oil |
| CN104178210A (en) * | 2013-05-27 | 2014-12-03 | 山东恒导石油化工股份有限公司 | Method and technological apparatus for recovering waste high-boiling-point heat-transfer oil |
| CN103351939A (en) * | 2013-06-28 | 2013-10-16 | 姜皓 | Refine and regeneration method of waste lubricant oil and regeneration device thereof |
| CN103351939B (en) * | 2013-06-28 | 2015-01-21 | 姜皓 | Refine and regeneration method of waste lubricant oil and regeneration device thereof |
| CN104531324A (en) * | 2014-11-28 | 2015-04-22 | 刘林 | Method for producing gear lubricating oil by using recovered lubricating oil |
| CN104560354A (en) * | 2014-12-24 | 2015-04-29 | 惠州Tcl环境科技有限公司 | Method and system for recycling and regenerating waste mineral oil |
| CN105001968A (en) * | 2015-06-30 | 2015-10-28 | 廖莱 | Technology for refining light and heavy lubricant base oil from waste engine oil |
| CN106147857A (en) * | 2016-08-19 | 2016-11-23 | 董琳 | A kind of environmentally friendly internal combustion engine used oil recycling technique |
| CN106693433A (en) * | 2017-02-04 | 2017-05-24 | 深圳市三环再生科技有限公司 | Waste lubricating oil regeneration distillation additive and application method thereof |
| CN107254329A (en) * | 2017-07-12 | 2017-10-17 | 宁波中循环保科技有限公司 | waste lubricating oil processing method |
| CN107254329B (en) * | 2017-07-12 | 2019-03-26 | 宁波中循环保科技有限公司 | Waste lubricating oil processing method |
| CN107353996A (en) * | 2017-07-31 | 2017-11-17 | 奇台县佳浩工程建设有限公司 | Waste lubricant oil regeneration utilization process and its process units |
| CN109233988A (en) * | 2018-08-06 | 2019-01-18 | 天津大学 | The clean high-valued recycling and reusing method and apparatus of waste lubricating oil |
| CN108998091A (en) * | 2018-09-12 | 2018-12-14 | 山东齐创石化工程有限公司 | Waste mineral oil regeneration technique |
| CN108998091B (en) * | 2018-09-12 | 2019-08-23 | 山东齐创石化工程有限公司 | Waste mineral oil regeneration technique |
| CN118594531A (en) * | 2024-05-30 | 2024-09-06 | 重庆工商大学 | Waste wind power lubricating oil hydrogenation catalyst, preparation method and application |
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