CN102433212A - Method and device for purifying waste lubricating oil - Google Patents
Method and device for purifying waste lubricating oil Download PDFInfo
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- CN102433212A CN102433212A CN2011103188432A CN201110318843A CN102433212A CN 102433212 A CN102433212 A CN 102433212A CN 2011103188432 A CN2011103188432 A CN 2011103188432A CN 201110318843 A CN201110318843 A CN 201110318843A CN 102433212 A CN102433212 A CN 102433212A
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- lubricating oil
- waste lubricating
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- oil
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- 239000010687 lubricating oil Substances 0.000 title claims abstract description 102
- 239000002699 waste material Substances 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 61
- 239000002199 base oil Substances 0.000 claims abstract description 36
- 238000000746 purification Methods 0.000 claims abstract description 24
- 239000010409 thin film Substances 0.000 claims abstract description 22
- 238000001704 evaporation Methods 0.000 claims abstract description 21
- 230000008020 evaporation Effects 0.000 claims abstract description 21
- 238000001179 sorption measurement Methods 0.000 claims abstract description 19
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 17
- 238000000526 short-path distillation Methods 0.000 claims description 19
- 238000010521 absorption reaction Methods 0.000 claims description 11
- 229930195733 hydrocarbon Natural products 0.000 claims description 11
- 150000002430 hydrocarbons Chemical class 0.000 claims description 11
- 238000002203 pretreatment Methods 0.000 claims description 10
- 239000004215 Carbon black (E152) Substances 0.000 claims description 8
- 238000007701 flash-distillation Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 235000015110 jellies Nutrition 0.000 claims description 6
- 239000008274 jelly Substances 0.000 claims description 6
- 238000009987 spinning Methods 0.000 claims description 6
- 238000007781 pre-processing Methods 0.000 claims description 5
- 239000002594 sorbent Substances 0.000 claims description 4
- 238000000199 molecular distillation Methods 0.000 abstract description 4
- 238000007670 refining Methods 0.000 abstract description 2
- 230000000295 complement effect Effects 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 18
- 239000000470 constituent Substances 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000295 fuel oil Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 229910017709 Ni Co Inorganic materials 0.000 description 2
- 229910003267 Ni-Co Inorganic materials 0.000 description 2
- 229910003262 Ni‐Co Inorganic materials 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 229910003296 Ni-Mo Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000004375 physisorption Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to a purification method of waste lubricating oil, which organically combines the technical processes of waste lubricating oil pretreatment, adsorption treatment, thin film evaporation, molecular distillation, hydrogenation complementary refining and the like, improves the yield of base oil, and improves the quality of the base oil.
Description
Technical field
The present invention relates to a kind of method of purification and device thereof of waste lubricating oil.More specifically, the present invention provides a kind of steps such as pre-treatment, adsorption treatment, thin film evaporation, short-path distillation and hydrofinishing, method of the I that from waste lubricating oil, purifies, II class base oil of successively waste lubricating oil being carried out.
Background technology
Lubricating oil is widely used in the industries such as manufacturing, plastics, chemical industry, transportation, and along with the fast development of industrial technology, and its demand and consumption also increased day by day.Therefore, purification and the utilization to waste lubricating oil has important environment and economic function.
Conventional waste lubricating oil method of purification generally includes: through alkali cleaning waste lubricating oil is carried out pre-treatment; Carry out molecular distillation and remove the moisture in the waste lubricating oil; To carry out carclazyte absorption through the waste lubricating oil after the molecular distillation; Outgas and decolour.Carry out pre-treatment through alkali cleaning, can produce the part alkaline residue and remain in the lubricating oil component, the salt that generates simultaneously is not easy from waste lubricating oil, to separate, and efficient is low and can not remove the moisture in the waste lubricating oil efficiently.After molecular distillation, carry out carclazyte absorption, in the process of the degassing and decolouring, can lose a large amount of base oils, thereby base oil yield is reduced.
Summary of the invention
The technical problem that the application will solve is to provide a kind of method of purification of waste lubricating oil, improves the yield of base oil, improves the quality of base oil simultaneously.
According to an embodiment of the invention, a kind of method of purification of waste lubricating oil is provided, said method comprises carries out steps such as pre-treatment, adsorption treatment, thin film evaporation and short-path distillation successively to waste lubricating oil.Waste lubricating oil is carried out pre-treatment, to remove mechanical impurity and the moisture in the said waste lubricating oil; To carrying out adsorption treatment, to remove additive and the jelly in the said waste lubricating oil through said pretreated waste lubricating oil; Waste lubricating oil to through said adsorption treatment carries out thin film evaporation, to slough residual micro-moisture and light hydrocarbon component; Waste lubricating oil to through said thin film evaporation carries out short-path distillation, to isolate the base oil fractions in the said waste lubricating oil.
According to an embodiment of the invention, said preprocessing process comprises spinning and flash distillation.
According to another implementation of the invention, sorbent used in the said adsorption treatment process is carclazyte, and oily temperature wherein is 150～170 ℃, and the consumption of said carclazyte is 3～5wt% of waste lubricating oil weight.
According to another implementation of the invention, the temperature of said thin film evaporation process is 170～190 ℃, and psia is 200～300Pa.
According to another embodiment; Said short-path distillation process comprises parallel connection or placed in-line three-stage distillation; And the temperature of said three-stage distillation is respectively 190～220 ℃, 220～240 ℃, 240～280 ℃, and psia is respectively 30～60Pa, 10～30Pa, 1～10Pa.
According to an embodiment of the invention, the method for purification of said waste lubricating oil further comprises carries out hydrofinishing to the lubricating oil after handling through said short-path distillation.
According to another embodiment of the present invention, a kind of purifying plant of waste lubricating oil is provided, comprise the separating centrifuge, flash tank, absorption reaction jar, thin-film evaporator, the molecular still that connect successively, and optional hydrogenation fixed-bed reactor.
Utilize waste lubricating oil method of purification of the present invention that the yield of base oil is improved, improve the base oil quality simultaneously.Oil product through producing after the short-path distillation process can meet I class base oil standard; Further the oil product through producing after the hydrofinishing can meet II class base oil standard.
Description of drawings
Fig. 1 is the process flow sheet according to the waste lubricating oil method of purification of embodiment of the present invention.
Embodiment
The invention provides a kind of method of purification of waste lubricating oil, comprising: waste lubricating oil is carried out pre-treatment, to remove mechanical impurity and the moisture in the waste lubricating oil; To carrying out adsorption treatment, remove additive and jelly in the waste lubricating oil through pretreated waste lubricating oil; Waste lubricating oil to through adsorption treatment carries out thin film evaporation, sloughs residual micro-moisture and light hydrocarbon component; Waste lubricating oil to through thin film evaporation carries out short-path distillation, isolates the base oil fractions in the said waste lubricating oil.
Below will specify the method for purification of above-mentioned waste lubricating oil with reference to Fig. 1.
The method of purification of waste lubricating oil of the present invention comprises processes such as pre-treatment, adsorption treatment, thin film evaporation and short-path distillation.Simultaneously, in order to improve the base oil quality, aforesaid method can further comprise the hydrofinishing process.
Below will set forth in detail each process in the above-mentioned method of purification with reference to Fig. 1.
Pre-treatment
Preprocessing process generally includes spinning and flash vaporization process.Waste lubricating oil pumps into separating centrifuge from head tank, to remove most of mechanical impurity.Usually the rotating speed of setting separating centrifuge is that 1440rpm, power are 11kw.Waste lubricating oil after the spinning gets into flash tank after preheater is heated to 90 ℃.Through the flash condenser condensation, the liquid phase that condensation goes out gets into water distributing can as gas phase for the water vapour that removes after the flash distillation and a small amount of light constituent hydro carbons, and isolated light constituent hydrocarbon fuel oil pumps into fuel oil drum through the light oil pump.Flash distillation remove the liquid waste lubricating oil that stays behind the moisture by flash tank at the bottom of pump pump, filter the raw material that the back is used as adsorption process through strainer.
Removed most of mechanical impurity and the free water content in the waste lubricating oil through this preprocessing process, prepared for waste lubricating oil gets into Distallation systm.
Adsorption process
Adsorption process is to utilize the physisorption of sorbent material to remove additive and jelly in the waste lubricating oil.Sorbent material commonly used is a carclazyte for example, but is not limited thereto.Adsorption process is carried out in the absorption reaction jar.
Carclazyte is pumped into carclazyte absorption reaction jar after metering from the carclazyte storage tank; The ratio of carclazyte is 3～5wt% of waste lubricating oil weight; When stirring, make waste lubricating oil be warming up to 150～170 ℃; Make carclazyte contact absorption more fully with oil product, through carclazyte absorption to remove most of additive and the jelly etc. in the waste lubricating oil.After the contact absorption 1～2 hour, waste lubricating oil for example is pumped to filtration unit such as filter press device and filters the raw material of back as the thin film evaporation process.
Thin film evaporation
The waste lubricating oil of handling through adsorption process is preheating to entering thin-film evaporator evaporation more than 150 ℃ through interchanger; To slough residual micro-moisture and light hydrocarbon component; Vaporization temperature in the thin-film evaporator is generally 170～190 ℃, and psia is generally 200～300Pa.Light constituent is an oil fuel, mainly is diesel oil distillate, removes the raw material of the remaining ingredient of light constituent as next step molecular still.
Can remove minute quantity moisture and boiling point in the waste lubricating oil at the light hydrocarbon component below 350 ℃ through this thin film evaporation process, thereby, guarantee that basic oil flash, viscosity and the viscosity index produced meet the base oil standard for short-path distillation provides qualified raw material.
Short-path distillation
The waste lubricating oil of handling through the thin film evaporation process gets into and comprises parallel connection or placed in-line three grades of molecular stills, and according to the requirements such as component characteristic of raw material, 3 molecular stills can be connected into three grades, or parallelly connected with 1 after 2 series connection, or 3 and be unified into one-level.During series connection, first isolated heavy constituent of molecular still directly gets into second molecular still and further separates, and second isolated heavy constituent of molecular still directly gets into the 3rd molecular still and further separate.Isolated in every molecular still is base oil fractions than light constituent, therefore can obtain three kinds of base oil fractions and heavy constituent oil fuel.During the parallel connection of base oil fractions equipment, can produce one or both base oil fractions and heavy constituent oil fuel.The three-stage distillation temperature is respectively: 190～220 ℃, 220～240 ℃, 240～280 ℃.Three grades of psia are respectively: 30～60Pa, 10～30Pa, 1～10Pa.
This short-path distillation process is thoroughly isolated the base oil fractions in the waste lubricating oil component, and guarantees the fine quality of base oil.
Hydrofinishing
The base oil that comes out through short-path distillation can further carry out hydrofinishing, and this hydrofinishing process is for example being carried out in the hydrogenation fixed-bed reactor usually.The base oil that will pass through short-path distillation pumps in the hydrogenation fixed-bed reactor, uses the hydrogenation catalyst commonly used of waste oil regeneration to carry out hydrofining reaction, makes born again lubricant base meet the national standard of lubricant base fully.Hydrogenation catalyst commonly used can for example be Ni-Co/Al
2O
3Type or Ni-Mo/Al
2O
3Type, the loadings of hydrogenation catalyst are 1.2kg/ ton oil plant.Above-mentioned hydrofining reaction preferably carries out under the pressure of 350 ℃ temperature, 13MPa, and the reactor drum empty tower gas velocity is 0.2m/s.
Oil product through producing after the short-path distillation technology meets I class base oil standard; If the base oil that produces is further passed through hydrofinishing, can obtain standard compliant II class base oil.The output capacity of base oil was about 60% after conventional waste lubricating oil method of purification was purified.And this mode of employing waste lubricating oil of purifying, waste oil is about 72% through the output capacity of the back base oil of purifying.
Embodiment
Waste lubricating oil (performance is as shown in table 1) is pumped into centrifuge separator from head tank, be of a size of 1850 (L) x1300 (W) x1250 (H), centrifuge speed is that 7500rpm, power are 11kw.Waste lubricating oil after the spinning gets into flash tank after preheater is heated to 90 ℃.The water vapour that removes after the flash distillation is with the light constituent hydro carbons is through the flash condenser condensation on a small quantity, and the liquid phase that condensation goes out gets into water distributing can, and isolated oil fuel pumps into fuel oil drum through the light oil pump, and uncooled gas is extracted out by the vacuum unit.Waste lubricating oil after the flash distillation by flash tank at the bottom of pump pump, filter back entering tundish 1 through strainer.
Waste lubricating oil gets into carclazyte absorption reaction jar from tundish 1, and the carclazyte adding proportion is the 4wt% of waste lubricating oil weight, makes waste lubricating oil be warming up to 160 ℃ through stirring.Contact absorption after 1 hour, waste lubricating oil gets into tundish 2 after filtration unit filters.
The waste lubricating oil of tundish 2 is preheating to 150 ℃ of entering thin-film evaporator evaporations through interchanger, and the temperature of film evaporator is 180 ℃, and psia is generally 200Pa.Waste lubricating oil after evaporation gets into tundish 3.
Waste lubricating oil pumps into three grades of placed in-line molecular stills through tundish 3, and its temperature is respectively 200 ℃, 230 ℃, 260 ℃, and pressure is respectively 45Pa, 20Pa, 5Pa.The base oil that obtains reclaiming is separated in the distillation back, and its each item performance test results is shown in Table 1.
Base oil through short-path distillation comes out can further be used Ni-Co/Al in the hydrogenation fixed-bed reactor
2O
3The type hydrogenation catalyst carries out hydrofinishing, and temperature is that 350 ℃, pressure are that 13MPa and empty tower gas velocity are 0.2m/s in the hydrogenation fixed-bed reactor, and the loadings of hydrogenation catalyst is a 1.2kg/ ton oil plant.Base oil each item performance test results after refining is shown in Table 1.
Comparative Examples
Get 50m
3Waste lubricating oil (performance is as shown in table 1) adds the NaOH solution of 100L 50% to it, stirs and is warming up to 60 ℃.After the sedimentation 24 hours, be cooled to room temperature, and filter.Waste lubricating oil after filtering is preheating to 150 ℃ of entering thin-film evaporator evaporations, and the temperature of film evaporator is 180 ℃, and psia is generally 200Pa.To be warmed up to 120～140 ℃ through the waste lubricating oil after the evaporation; Constant temperature with stir adding carclazyte down (its consumption be about oil mass 4%); After adding carclazyte, continue to stir half a hour, leave standstill a night at 110～120 ℃ of following constant temperature; Second day filtered while hot, and promptly obtain the lubricating oil that reclaims through the degassing and decolouring.Lube oil yield and performance that test is reclaimed are as shown in table 1.
Table 1
Can find out by table 1; Reclaim the base oil that obtains according to the method for embodiment, do not have the viscosity ratio hydrogenation before the hydrogenation after viscosity high, this is owing to have the part macromolecular cleavage to become small molecules in the hydrogenation process; The part cyclic hydrocarbon becomes straight-chain paraffin or alkene; The phenyl ring open chain, molecular weight diminishes, and saturation ratio improves.And behind the hydrogenation, it mainly is because the cause that the saturation ratio of hydrocarbon improves that viscosity index uprises; The major cause of flash-point step-down is that the part macromolecular cleavage becomes small molecules, causes flash-point to reduce; Depression of pour point is that zero pour is just high more because the cerul in the oil product is high more, and the cerul molecular chain is broken behind the hydrogenation, by saturated reason; It mainly is that the hydro carbons saturation ratio improves that oxidation stability uprises, and removes sulfide and nitride, oxide compound, and the oil product resistance of oxidation is improved.
Therefore; Compare with the method for Comparative Examples; Method according to the embodiment of the invention is carried out pre-treatment, and the spinning of employing and flash distillation preprocessing process can more effectively be removed the moisture in the waste lubricating oil, and does not adopt alkali cleaning and can in lubricating oil component, not produce alkaline residue residual; Adjusted adsorption process simultaneously and carried out opportunity, made that the organic efficiency of base oil is high, quality is better.
Claims (11)
1. the method for purification of a waste lubricating oil comprises:
Waste lubricating oil is carried out pre-treatment, to remove mechanical impurity and the moisture in the said waste lubricating oil;
To carrying out adsorption treatment, to remove additive and the jelly in the said waste lubricating oil through said pretreated waste lubricating oil;
Waste lubricating oil to through said adsorption treatment carries out thin film evaporation, to slough residual micro-moisture and light hydrocarbon component; And to carrying out short-path distillation, to isolate the base oil fractions in the said waste lubricating oil through the waste lubricating oil of said thin film evaporation;
, above step obtains output capacity after purifying and is 72 ± 2% base oil, in the gross weight of said waste lubricating oil.
2. the method for purification of waste lubricating oil according to claim 1, wherein said preprocessing process comprises spinning and flash distillation, is respectively applied for mechanical impurity and the moisture removed in the said waste lubricating oil.
3. the method for purification of waste lubricating oil according to claim 1, sorbent used in the wherein said adsorption treatment process is carclazyte.
4. the method for purification of waste lubricating oil according to claim 3, the consumption of wherein said carclazyte is 3～5wt% of said waste lubricating oil weight.
5. the method for purification of waste lubricating oil according to claim 1, oily temperature is 150～170 ℃ in the wherein said adsorption treatment process.
6. the method for purification of waste lubricating oil according to claim 1, the temperature of wherein said thin film evaporation process is 170～190 ℃, psia is 200～300Pa.
7. the method for purification of waste lubricating oil according to claim 1, wherein said short-path distillation process comprise parallel connection or placed in-line three-stage distillation.
8. the method for purification of waste lubricating oil according to claim 7, the temperature of wherein said three-stage distillation is respectively 190～220 ℃, 220～240 ℃, 240～280 ℃, and psia is respectively 30～60Pa, 10～30Pa, 1～10Pa.
9. the method for purification of waste lubricating oil according to claim 1 further comprises the lubricating oil after handling through said short-path distillation is carried out hydrofinishing.
10. the purifying plant of a waste lubricating oil comprises successively:
Separating centrifuge is to remove the mechanical impurity in the said waste lubricating oil;
Flash tank is to remove the moisture in the said waste lubricating oil;
The absorption reaction jar is to remove additive and the jelly in the said waste lubricating oil;
Thin-film evaporator is to slough residual micro-moisture and light hydrocarbon component;
And molecular still, to isolate the base oil fractions in the said waste lubricating oil.
11. the purifying plant of waste lubricating oil according to claim 10 further comprises the hydrogenation fixed-bed reactor behind said molecular still, the lubricating oil after handling through short-path distillation is carried out hydrofinishing.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102719266A (en) * | 2012-07-03 | 2012-10-10 | 宁波博汇石油化工有限公司 | Heavy oil short-path distillation (molecular distillation) continuous production process |
| CN103058303A (en) * | 2012-11-26 | 2013-04-24 | 北京化工大学 | Method for separating inorganic salt substances from high-salt liquid waste |
| CN103285734A (en) * | 2013-06-25 | 2013-09-11 | 深圳市森科妍科技有限公司 | A treatment process and a system for waste organic solvents based on nano filter membranes |
| CN103820200A (en) * | 2014-01-28 | 2014-05-28 | 连力生 | Process for regenerating base oil from waste lubricating oil |
| CN103849454A (en) * | 2014-01-28 | 2014-06-11 | 连力生 | Device for regenerating base oil by utilizing waste lubrication oil |
| CN104611058A (en) * | 2015-02-05 | 2015-05-13 | 武汉科林精细化工有限公司 | Hydrofining process of waste lubricating oil |
| CN105572053A (en) * | 2015-12-30 | 2016-05-11 | 中国神华能源股份有限公司 | Removal method and analysis method of impurities in lubricating oil sample in mining device oil fluid monitoring spectral analysis |
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| CN102719266A (en) * | 2012-07-03 | 2012-10-10 | 宁波博汇石油化工有限公司 | Heavy oil short-path distillation (molecular distillation) continuous production process |
| CN103058303A (en) * | 2012-11-26 | 2013-04-24 | 北京化工大学 | Method for separating inorganic salt substances from high-salt liquid waste |
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| CN103849454A (en) * | 2014-01-28 | 2014-06-11 | 连力生 | Device for regenerating base oil by utilizing waste lubrication oil |
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