CN102504933B - Regeneration method of waste lubricating oil - Google Patents
Regeneration method of waste lubricating oil Download PDFInfo
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- CN102504933B CN102504933B CN 201110365025 CN201110365025A CN102504933B CN 102504933 B CN102504933 B CN 102504933B CN 201110365025 CN201110365025 CN 201110365025 CN 201110365025 A CN201110365025 A CN 201110365025A CN 102504933 B CN102504933 B CN 102504933B
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- oil
- lubricating oil
- waste lubricating
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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 further investigation and the development of Technology of Used Lube Oil Regeneration, the treatment capacity of the industrialized unit of waste lubricant oil regeneration is also increasing, and is therefore also more and more higher to environmental requirement." process engineering for regenerating of waste lubricating oil " (patent No.: ZL200610086926.2) few, simple to operate, the good product quality of the clay treatment process facility investment adopted of patent is the first-selected process for purification of middle-size and small-size regenerator for waste lubricating oil.When the treatment capacity of regenerator for waste lubricating oil 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.Hydrofining is a kind of cleaning procedure, does not produce the oil-containing argil slag, and the quality of lube base oil production is good, yield also increases.The present invention is used for waste lubricant oil regeneration with autonomous improved hydrofining technology and processes, and provides the advanced technologies technology of clean environment firendly more for building large-scale regenerator for waste lubricating oil.
Process in practice at waste lubricant oil regeneration and find, the waste lubricating oil raw material type of collection is many, composition is complicated, and some inferior raw material even affects the normal operation of subsequent technique.Therefore, improve for pretreatment technology, make this Technology wider to the subject range of raw material.
Summary of the invention
The objective of the invention is improve to improve and expansion " Technology of Used Lube Oil Regeneration " patent (patent No.: ZL200610086926.2), provide that a kind of scope of application is wider, the method for regenerating waste lubricating oil of environmental protection more.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of method for regenerating waste lubricating oil is provided, comprises at least the several steps of waste oil pre-treatment, short-path distillation and hydrofining, concrete steps are as follows:
(1) waste oil pre-treatment: waste lubricating oil is placed in the mixing tank that a band stirs, the basic cpd that adds waste lubricating oil weight 0-5.0%, stirred 10-60 minute under room temperature to 100 ℃ condition, then moved into the slurry tank sedimentation 1-10 hour, the basic cpd that preferably adds waste lubricating oil weight 0.5～1.0%, stirred under 60～90 ℃ 20～40 minutes, then sedimentation is 10 hours, the basic cpd that most preferably adds waste lubricating oil weight 0.5-1.0%, stirred 40 minutes at 90 ℃ of temperature, then sedimentation is 10 hours, to remove moisture and impurity;
(2) short-path distillation: the waste oil that step (1) was processed enters short-path distillation, at least will pass through successively following two-step distillation: first step short-path distillation fractionates out the light lubricating oil oil base stock, operational condition is temperature 150-250 ℃, vacuum tightness 30-100Pa; Preferred operational condition is: temperature 170-200 ℃, and vacuum tightness 30-50Pa; Then material enters second stage short-path distillation and steams middle matter lube oil base stocks, and Residual oil is discharged at the bottom of by tower, and its operational condition is temperature 180-260 ℃, vacuum tightness 5-20Pa; The preferred operations condition is temperature 200-230 ℃, vacuum tightness 5-10Pa.
(3) hydrofining: the various lube oil base stocks that distill out through step (2) enter respectively hydro-refining unit, react under hydrogenation catalyst catalysis, 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 thus trace impurity and decolouring in oil product, produce the high quality lubricant base.
Method of the present invention preferably after pre-treatment and short-path distillation take a step forward and comprise rectification step, be about to the pretreated waste oil of step (1) and enter after filtering rectifying tower, 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 with this water and/or light Fuel that contains in waste lubricating oil.
The described basic cpd of step (1) can be one or more the mixture in inorganic alkaline compound or organic basic compound; The mixture of one or more in preferred sodium hydroxide, calcium hydroxide or alcamines or 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 that described second stage short-path distillation steams after middle matter lube oil base stocks enters third stage short-distance distiller, 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.
The described Hydrobon catalyst of step (3) can chosen from Fe-Molybdenum catalyzer or the Hydrobon catalyst of the type such as Cobalt-Molybdenum catalyzer.
The present invention is a kind of combination process, simple, the easy row of method, equipment used is all 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 process various waste lubricating oils, and have the beneficial effect of following several respects:
1. compared with prior art, method for regenerating waste lubricating oil of the present invention has adopted hydrorefined step, and the characteristics of hydrogenation process are without 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 the prior art, technique 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 larger Social benefit and economic benefit.
Embodiment
Further illustrate characteristics of the present invention below by specific examples.
Embodiment 1.
The present embodiment waste lubricating oil character used sees Table 1.
The 10kg waste lubricating oil is passed through steps of processing:
(1) pre-treatment
Waste lubricating oil is placed in the mixing tank that a band stirs, stirred 20 minutes under 60 ℃ of conditions, then moved into the slurry tank sedimentation 10 hours, remove moisture and mechanical impurity;
(2) rectifying:
The pretreated waste oil of step (1) is entered 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 processed enters short-path distillation, passes through successively following three-stage distillation: first step short-path distillation operational condition is temperature 170-200 ℃, vacuum tightness 30-50Pa, fractionates out the light lubricating oil oil base stock; Then material enters second stage short-path distillation, its operational condition is temperature 200-230 ℃, vacuum tightness 5-10Pa, steam middle matter lube oil base stocks, then material enters third stage short-distance distiller, 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) hydrofining:
Through step (3) distill out light, in and the heavy grease oil base stock enter respectively hydro-refining unit, react under iron-Molybdenum catalysts, its main operational 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 thus trace impurity and decolouring in oil product, obtain three kinds of lube base oil productions of HVI100, HVI200 and HVI350, three kinds of product properties see Table 2.
The character of table 1 waste lubricating oil raw material
| 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
As can be seen from Table 2, 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 10% left and right with " process engineering for regenerating of waste lubricating oil ".
Embodiment 2
The present embodiment waste lubricating oil character used sees Table 3.
The 10kg waste lubricating oil is passed through steps of processing:
(1) pre-treatment:
Waste lubricating oil is placed in the mixing tank that a band stirs, and the nitrogen content that adds by weight percentage waste lubricating oil weight 0.5-1.0% is at 40～41% mixing ethyleneamines.Stirred 40 minutes under 90 ℃ of conditions, then moved into the slurry tank sedimentation 10 hours, remove moisture and impurity.
(2) rectifying:
The pretreated waste oil of step (1) is entered 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 processed enters short-path distillation, passes through successively following three-stage distillation: 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) hydrofining:
The lubricant base that distills out through step (3) enters respectively hydro-refining unit, 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 and three kinds of lube base oil productions of HVI350, its character sees 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, illustrates that this waste oil deterioration by oxidation is serious, is a typical waste lubricating oil raw material inferior.
As can be seen from Table 4, through three kinds of lube base oil production HVI100 of the present embodiment method processing treatment, HVI200 and HVI350 have all reached China's all-purpose engine oil base oil standard.
Due to water-content in the waste lubricating oil raw material and the light Fuel component concentration all higher, in waste oil, the lubricating oil component actual content is lower, so the productive rate of lube base oil production is also low than embodiment 1.
Renovation process by embodiment 2 explanation waste lubricating oils provided by the invention can manipulation of regeneration waste lubricating oil raw material inferior.
Claims (8)
1. a method for regenerating waste lubricating oil, is characterized in that, comprises at least following step:
(1) waste oil pre-treatment: waste lubricating oil is placed in the mixing tank that a band stirs, the basic cpd that adds waste lubricating oil weight 0-5.0%, stirred 10-60 minute under room temperature to 100 ℃ condition, then moved into the slurry tank sedimentation 1-10 hour, to remove moisture and impurity;
(2) short-path distillation: the waste oil that step (1) was processed enters short-path distillation, passes through at least successively following two-step distillation: first step short-path distillation operational condition is temperature 150-250 ℃, vacuum tightness 30-100Pa, fractionates out the light lubricating oil oil base stock; Then material enters second stage short-path distillation, and its operational condition is temperature 180-260 ℃, vacuum tightness 5-20Pa, steams middle matter lube oil base stocks, and Residual oil is discharged at the bottom of by tower;
(3) hydrofining: the various lube oil base stocks that distill out through step (2) enter respectively hydro-refining unit, react under hydrogenation catalyst catalysis, catalyzer is selected from iron-molybdenum catalyst or cobalt-molybdenum catalyzer, its main operational 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 thus trace impurity and decolouring in oil product, produce the high quality lubricant base.
2. method for regenerating waste lubricating oil claimed in claim 1, it is characterized in that: taking a step forward with short-path distillation after pre-treatment comprises rectification step, be about to the pretreated waste oil of step (1) and enter after filtering rectifying tower, its operational condition: temperature is that 130-200 ℃, vacuum tightness are 150-350Pa, to remove water and/or the light Fuel that contains in waste lubricating oil.
3. method for regenerating waste lubricating oil claimed in claim 2 is characterized in that: described rectifying tower operational condition is that temperature 150-170 ℃, vacuum tightness are 240-260Pa.
4. method for regenerating waste lubricating oil claimed in 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 ethyleneamines compounds.
5. method for regenerating waste lubricating oil claimed in 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 at 90 ℃ of temperature, then sedimentation is 10 hours.
6. method for regenerating waste lubricating oil claimed in 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. method for regenerating waste lubricating oil claimed in claim 1, it is characterized in that: further comprise third stage short-path distillation in the short-path distillation of step (2), be that the material that described second stage short-path distillation steams after middle matter lube oil base stocks enters third stage short-distance distiller, 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. method for regenerating waste lubricating oil claimed in claim 7, it is characterized in that: described third stage short-distance distiller operational condition is: temperature 230-250 ℃, vacuum tightness 4-6Pa.
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|---|---|---|---|
| CN 201110365025 CN102504933B (en) | 2011-11-17 | 2011-11-17 | Regeneration method of waste lubricating oil |
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|---|---|---|---|
| CN 201110365025 CN102504933B (en) | 2011-11-17 | 2011-11-17 | Regeneration method of waste lubricating oil |
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| CN102504933B true CN102504933B (en) | 2013-05-15 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104178210B (en) * | 2013-05-27 | 2018-08-03 | 山东恒利热载体工程技术有限公司 | The method and process unit of higher boiling conduction oil are discarded in a kind of recycling |
| 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 |
| CN106147857B (en) * | 2016-08-19 | 2018-11-20 | 广州恒滤环保科技有限公司 | 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 |
| 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 |
| 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 |
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