CN110257153A - Waste lubricating oil environment protection regeneration method - Google Patents
Waste lubricating oil environment protection regeneration method Download PDFInfo
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- CN110257153A CN110257153A CN201910615994.0A CN201910615994A CN110257153A CN 110257153 A CN110257153 A CN 110257153A CN 201910615994 A CN201910615994 A CN 201910615994A CN 110257153 A CN110257153 A CN 110257153A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/82—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74 characterised by the presence of specified groups, e.g. introduced by chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0016—Working-up used lubricants to recover useful products ; Cleaning with the use of chemical agents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0025—Working-up used lubricants to recover useful products ; Cleaning by thermal processes
- C10M175/0033—Working-up used lubricants to recover useful products ; Cleaning by thermal processes using distillation processes; devices therefor
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0025—Working-up used lubricants to recover useful products ; Cleaning by thermal processes
- C10M175/0041—Working-up used lubricants to recover useful products ; Cleaning by thermal processes by hydrogenation processes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0083—Lubricating greases
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Abstract
The present invention relates to waste lubricating oil processing technology fields, and in particular to waste lubricating oil environment protection regeneration method, comprising the following steps: pretreatment, UF membrane, hydrofinishing.Pretreated waste lubricating oil is passed through first order membrane module by the present invention under the conditions of supercritical carbon dioxide, supercritical carbon dioxide can make the viscosity of waste lubricating oil reduce 80% or more, improve Membrane Filtration Flux, enter back into second level membrane module, second level membrane module is compound membrane module of receiving, have the characteristics that Membrane Filtration Flux is big, entire technical process does not aoxidize, it does not decompose, waste water, waste liquid and exhaust gas are not generated, no pollution to the environment, it is environmentally protective, and the comprehensive utilization ratio of waste lubricating oil is up to 90% or more.
Description
Technical field
The present invention relates to waste lubricating oil processing technology fields, and in particular to waste lubricating oil environment protection regeneration method.
Background technique
With the rapid development of mechanical industry, for applying the demand for lubricating oil between each components constantly to expand, and
Petroleum resources are increasingly in short supply, and waste oil regeneration becomes the strategic project developed a circular economy.There is only various in waste lubricating oil
Oxidation product, it is also non-ideal containing moisture, metallic particles, carbon granule, dust, greasy filth, additive, residue pitch and mechanical admixture etc.
Component seriously affects each process of refining waste lubricating oil following process.
In recent years, membrane separation process in waste lubricating oil using more, which has easy to operate, and equipment can be small-sized
Change, the high and low energy consumption of separative efficiency and it is environmental-friendly the features such as, but that there are filtration fluxs is small, the suitable membrane aperture size of selection and
The problems such as suitable membrane material.In consideration of it, providing a kind of waste lubricating oil environment protection regeneration method regarding to the issue above.
Summary of the invention
The purpose of the present invention is to provide a kind of waste lubricating oil environment protection regeneration methods, and this method is with Membrane Filtration Flux
Big feature, entire technical process are not aoxidized, are not decomposed, and do not generate waste water, waste liquid and exhaust gas, no pollution to the environment, green ring
It protects, and the comprehensive utilization ratio of waste lubricating oil is up to 90% or more.
To achieve the goals above, the invention provides the following technical scheme:
Waste lubricating oil environment protection regeneration method, the following steps are included:
S1: each component and physicochemical property of waste lubricating oil are analyzed in pretreatment, qualitative and quantitatively determine waste lubricating oil
In ideal composition and undesirable components；Flocculant is added into waste lubricating oil, demulsifier is added after stirring, is obtained after stirring
Mixture, mixture is settled by settling tank, and sedimentation time 10h takes upper layer waste lubricating oil；To upper layer waste lubricating oil into
Row vacuum distillation, isolates pretreated waste lubricating oil；
S2: pretreated waste lubricating oil is passed through first order membrane module by UF membrane under the conditions of supercritical carbon dioxide,
Enter back into second level membrane module；The membrane component of the first order membrane module is ceramic filtration membrane, the membrane element of the second level membrane module
Part is composite nanometer filtering film；
S3: the waste lubricating oil after UF membrane is reacted under catalysts conditions, further sloughs useless profit by hydrofinishing
The undesirable components such as all kinds of oxidation products and additive in lubricating oil obtain base oil and kerosene after air lift and drying, described to urge
Agent is molybdenum-Raney nickel or super steady H-Y type molecular sieve-aluminium oxide.
Preferably, the composite nanometer filtering film is by following steps processing preparation:
S1: preparing polyether sulfone basement membrane, polyether sulfone be dissolved in polyvinylpyrrolidone, and configuration is 30% containing mass fraction
Casting solution, 5-7h, and the standing and defoaming 2-3h in 45-50 DEG C of environment are stirred under the conditions of 45-50 DEG C, after being cooled to room temperature will
Casting solution is poured on knifing on glass, is put into film-forming in 10-25 DEG C of water-bath, is impregnated after removing from glass plate with deionized water
12-16h obtains polyether sulfone basement membrane, and is stored in spare in 10 DEG C of deionised waters；
S2: dispersing graphene oxide in deionized water, and the aqueous phase monomers solution that concentration is 1-15mg/L is made, will make
Standby polyether sulfone basement membrane is immersed in 40-60 minutes in aqueous phase monomers solution and takes out, and the water of polyether sulfone membrane surface is blotted with dryer
It is spare after phase monomer solution；
S3: n,N-Dimethylformamide is dissolved in acetylene, is configured the organic phase monomer solution of 1-5g/L, will be impregnated water
The polyether sulfone basement membrane of phase monomer solution is immersed in organic phase monomer solution, and temperature is to impregnate 5 minutes to take out at 20 DEG C, in baking oven
In handle 10 minutes under the conditions of 50 DEG C, obtain composite nanometer filtering film.
Preferably, the flocculant is that aluminium polychloride stirs at a temperature of 70 DEG C after flocculant is added into waste lubricating oil
Mix 2-4h.
Preferably, the demulsifier is that AR type demulsifier stirs at 50 °C after demulsifier is added into waste lubricating oil
Mix 1-3h.
Preferably, the vacuum distillation condition is 100 DEG C, and pressure is -0.5MPa.
It preferably, is 150MPa into the pressure of the first order membrane module, temperature is 40-60 DEG C, overcritical titanium dioxide
Carbon flow speed is 10~20m/s, and the pressure into the second level membrane module is 0.6MPa, and temperature is 80-90 DEG C.
Preferably, the pressure of the hydrofinishing is 0.5-1.0MPa, and temperature is 250-330 DEG C, hydrogen oil 800-1000, empty
Fast 3-3.5h-1。
The beneficial effects of the present invention are:
(1) waste lubricating oil environment protection regeneration method of the invention carries out each component to waste lubricating oil first and physicochemical property carries out
Analysis, it is qualitative and quantitatively determine ideal composition and undesirable components in waste lubricating oil, convenient for the system of subsequent treatment process condition
It is fixed, undesirable components are isolated, to protect ideal composition；It flocculated, be demulsified, settled and be evaporated under reduced pressure to waste lubricating oil again
Pretreating process, slough the water and impurity in waste lubricating oil；Waste lubricating oil is further processed in UF membrane, removes useless profit
Pretreated waste lubricating oil is passed through first by most of metal and additive in lubricating oil under the conditions of supercritical carbon dioxide
Grade membrane module, supercritical carbon dioxide can make the viscosity of waste lubricating oil reduce 80% or more, improve Membrane Filtration Flux, enter back into
Second level membrane module, second level membrane module be it is compound receive membrane module, have the characteristics that Membrane Filtration Flux is big；Finally by adding hydrogen smart
Technique processed further sloughs the undesirable components such as all kinds of oxidation products and additive in waste lubricating oil, after air lift and drying
To high-quality base oil and the good kerosene of by-product.
(2) each technique of the present invention is not aoxidized, is not decomposed when carrying out process to waste lubricating oil, is not generated waste water, is given up
Liquid and exhaust gas, no pollution to the environment is environmentally protective, and the regeneration rate of waste lubricating oil is up to 90% or more.
(3) present invention be attached on polyether sulfone basement membrane by amination graphene oxide prepare it is compound receive membrane module, because of oxygen
Hydroxyl, epoxy group are contained in graphite alkene surface, and there are carboxyl, and the specific surface area of super large in edge, use the oxidation stone of certain concentration
Black alkene prepares the polyether sulfone composite nanometer filtering film of doping amination graphene oxide by interfacial polymerization, which can improve
Common composite nanometer filter permeability of the membrane, selectivity and antifouling property, have the characteristics that Membrane Filtration Flux is big.
(4) material is easy to get in each technique of waste lubricating oil environment protection regeneration method of the invention, low in cost, has very high make
With value and good application prospect.
Detailed description of the invention
Fig. 1 is the step flow chart of waste lubricating oil environment protection regeneration method in the present invention.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
If technological means used is conventional hand well known to those skilled in the art without specified otherwise in following case study on implementation
Section.
Embodiment 1
In the present embodiment, the waste lubricating oil environment protection regeneration method, comprising the following steps:
S1: each component and physicochemical property of waste lubricating oil are analyzed in pretreatment, qualitative and quantitatively determine waste lubricating oil
In ideal composition and undesirable components；Aluminium polychloride is added into waste lubricating oil, stirs 4h at a temperature of 70 DEG C；After stirring
AR type demulsifier is added, 3h is stirred at 50 °C, obtains mixture after stirring, mixture is sunk by settling tank
Drop, sedimentation time 10h take upper layer waste lubricating oil；In 100 DEG C of temperature and under the conditions of pressure is -0.5MPa, to upper layer waste lubricating oil
It is evaporated under reduced pressure, isolates pretreated waste lubricating oil；
S2: pretreated waste lubricating oil is passed through first order membrane module by UF membrane under the conditions of supercritical carbon dioxide,
Pressure is 150MPa, and temperature is 60 DEG C, and stream of supercritical carbon dioxide speed is 20m/s, enters back into second level membrane module, pressure is
0.6MPa, temperature are 90 DEG C；The membrane component of the first order membrane module is ceramic filtration membrane, the membrane component of the second level membrane module
For composite nanometer filtering film；
S3: hydrofinishing reacts the waste lubricating oil after UF membrane, pressure 1.0MPa under catalysts conditions,
Temperature is 330 DEG C, hydrogen oil 1000, air speed 3.5h-1, further slough the unreasonablys such as all kinds of oxidation products and additive in waste lubricating oil
Think component, base oil and kerosene are obtained after air lift and drying, the catalyst is molybdenum-Raney nickel.
The composite nanometer filtering film is by following steps processing preparation:
S1: preparing polyether sulfone basement membrane, polyether sulfone be dissolved in polyvinylpyrrolidone, and configuration is 30% containing mass fraction
Casting solution, 7h, and the standing and defoaming 3h in 50 DEG C of environment are stirred under the conditions of 50 DEG C, is poured on casting solution after being cooled to room temperature
Knifing on glass is put into film-forming in 10 DEG C of water-baths, impregnates 16h with deionized water after removing from glass plate, obtains polyethers
Sulfuryl film, and be stored in spare in 10 DEG C of deionised waters；
S2: dispersing graphene oxide in deionized water, and the aqueous phase monomers solution that concentration is 1mg/L is made, will prepare
Polyether sulfone basement membrane is immersed in 60 minutes in aqueous phase monomers solution and takes out, and the aqueous phase monomers of polyether sulfone membrane surface are blotted with dryer
It is spare after solution；
S3: n,N-Dimethylformamide is dissolved in acetylene, is configured the organic phase monomer solution of 1g/L, will be impregnated water phase
The polyether sulfone basement membrane of monomer solution is immersed in organic phase monomer solution, and temperature is to impregnate 5 minutes to take out at 20 DEG C, in an oven
It is handled 10 minutes under the conditions of 50 DEG C, obtains composite nanometer filtering film.
Embodiment 2
Waste lubricating oil environment protection regeneration method is with embodiment 1 in the present embodiment, and details are not described herein, the difference is that, it is multiple
It is different to close nanofiltration membrane preparation condition.
The composite nanometer filtering film is by following steps processing preparation:
S1: preparing polyether sulfone basement membrane, polyether sulfone be dissolved in polyvinylpyrrolidone, and configuration is 30% containing mass fraction
Casting solution, 5h, and the standing and defoaming 2h in 45 DEG C of environment are stirred under the conditions of 45 DEG C, is poured on casting solution after being cooled to room temperature
Knifing on glass is put into film-forming in 25 DEG C of water-baths, impregnates 12h with deionized water after removing from glass plate, obtains polyethers
Sulfuryl film, and be stored in spare in 10 DEG C of deionised waters；
S2: dispersing graphene oxide in deionized water, and the aqueous phase monomers solution that concentration is 1mg/L is made, will prepare
Polyether sulfone basement membrane is immersed in 60 minutes in aqueous phase monomers solution and takes out, and the aqueous phase monomers of polyether sulfone membrane surface are blotted with dryer
It is spare after solution；
S3: n,N-Dimethylformamide is dissolved in acetylene, is configured the organic phase monomer solution of 1g/L, will be impregnated water phase
The polyether sulfone basement membrane of monomer solution is immersed in organic phase monomer solution, and temperature is to impregnate 5 minutes to take out at 20 DEG C, in an oven
It is handled 10 minutes under the conditions of 50 DEG C, obtains composite nanometer filtering film.
Embodiment 3
The preparation method is the same as that of Example 1 for composite nanometer filtering film in the present embodiment, and details are not described herein, the difference is that, profit of giving up
Each process conditions of lubricating oil environment protection regeneration method are different.
The waste lubricating oil environment protection regeneration method, the following steps are included:
S1: each component and physicochemical property of waste lubricating oil are analyzed in pretreatment, qualitative and quantitatively determine waste lubricating oil
In ideal composition and undesirable components；Aluminium polychloride is added into waste lubricating oil, stirs 2h at a temperature of 70 DEG C；After stirring
AR type demulsifier is added, 1h is stirred at 50 °C, obtains mixture after stirring, mixture is sunk by settling tank
Drop, sedimentation time 10h take upper layer waste lubricating oil；In 100 DEG C of temperature and under the conditions of pressure is -0.5MPa, to upper layer waste lubricating oil
It is evaporated under reduced pressure, isolates pretreated waste lubricating oil；
S2: pretreated waste lubricating oil is passed through first order membrane module by UF membrane under the conditions of supercritical carbon dioxide,
Pressure is 150MPa, and temperature is 40 DEG C, and stream of supercritical carbon dioxide speed is 10m/s, enters back into second level membrane module, pressure is
0.6MPa, temperature are 80 DEG C；The membrane component of the first order membrane module is ceramic filtration membrane, the membrane component of the second level membrane module
For composite nanometer filtering film；
S3: hydrofinishing reacts the waste lubricating oil after UF membrane, pressure 0.5MPa under catalysts conditions,
Temperature is 250 DEG C, hydrogen oil 800, air speed 3h-1, it is non-ideal further to slough all kinds of oxidation products and additive etc. in waste lubricating oil
Component, obtains base oil and kerosene after air lift and drying, and the catalyst is molybdenum-Raney nickel.
Embodiment 4
Waste lubricating oil environment protection regeneration method and composite nanometer filtering film preparation condition are with embodiment 2 in the present embodiment, herein no longer
It repeats, the difference is that, the Membrane Filtration Flux of composite nanometer filter film preparation is different.
The composite nanometer filtering film is by following steps processing graphene oxide and preparation:
S1: preparing polyether sulfone basement membrane, polyether sulfone be dissolved in polyvinylpyrrolidone, and configuration is 30% containing mass fraction
Casting solution, 5h, and the standing and defoaming 2h in 45 DEG C of environment are stirred under the conditions of 45 DEG C, is poured on casting solution after being cooled to room temperature
Knifing on glass is put into film-forming in 25 DEG C of water-baths, impregnates 12h with deionized water after removing from glass plate, obtains polyethers
Sulfuryl film, and be stored in spare in 10 DEG C of deionised waters；
S2: dispersing graphene oxide in deionized water, and the aqueous phase monomers solution that concentration is 10mg/L is made, will prepare
Polyether sulfone basement membrane is immersed in 60 minutes in aqueous phase monomers solution and takes out, and the aqueous phase monomers of polyether sulfone membrane surface are blotted with dryer
It is spare after solution；
S3: n,N-Dimethylformamide is dissolved in acetylene, is configured the organic phase monomer solution of 5g/L, will be impregnated water phase
The polyether sulfone basement membrane of monomer solution is immersed in organic phase monomer solution, and temperature is to impregnate 5 minutes to take out at 20 DEG C, in an oven
It is handled 10 minutes under the conditions of 50 DEG C, obtains composite nanometer filtering film.
Comparative example 1
The preparation method is the same as that of Example 1 for composite nanometer filtering film in the present embodiment, and details are not described herein, the difference is that, profit of giving up
Pretreated waste lubricating oil is directly passed through into first order membrane module in lubricating oil environment protection regeneration method.
Comparative example 2
Waste lubricating oil environment protection regeneration method is with embodiment 1 in the present embodiment, and details are not described herein, the difference is that, the
Second membrane module uses polyethersulfone membranes.
Comparative example 3
Waste lubricating oil environment protection regeneration method is with embodiment 1 in the present embodiment, and details are not described herein, the difference is that, the
Second membrane module uses n,N-Dimethylformamide filter membrane.
Comparative example 4
Waste lubricating oil environment protection regeneration method is with embodiment 1 in the present embodiment, and details are not described herein, the difference is that, the
Second membrane module is using n,N-Dimethylformamide and polyether sulfone composite filter membrane.
Table 1 is that the material performance of waste lubricating oil used in above-described embodiment is as follows:
Table 2 is that embodiment 1-4 and the comparing result of comparative example 1-4 are as follows in the present invention:
Table 3 is that the regeneration comprehensive utilization rate result of embodiment 1-4 and comparative example 1-4 in the present invention is as follows:
| Sample ID | Base oil yield | Kerosene yield | Total recovery |
| Embodiment 1 | 90.89% | 1.26% | 92.15% |
| Embodiment 2 | 89.03% | 1.18% | 90.21% |
| Embodiment 3 | 88.91% | 1.13% | 90.04% |
| Embodiment 4 | 92.07% | 1.41% | 93.48% |
| Comparative example 1 | 81.90% | 0.35% | 82.25% |
| Comparative example 2 | 83.16% | 0.41% | 83.57% |
| Comparative example 3 | 83.47% | 0.46% | 83.93% |
| Comparative example 4 | 84.51% | 0.55% | 85.06% |
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, all any modification, equivalent substitution, improvement and etc. be should all be included in the protection scope of the present invention.
Claims (7)
1. waste lubricating oil environment protection regeneration method, which comprises the following steps:
S1: each component and physicochemical property of waste lubricating oil are analyzed in pretreatment, qualitative and quantitatively determine in waste lubricating oil
Ideal composition and undesirable components；Flocculant is added into waste lubricating oil, demulsifier is added after stirring, is mixed after stirring
Object, mixture is settled by settling tank, and sedimentation time 10h takes upper layer waste lubricating oil；Upper layer waste lubricating oil is subtracted
Pressure distillation, isolates pretreated waste lubricating oil；
S2: UF membrane, by pretreated waste lubricating oil by the first order membrane module under the conditions of supercritical carbon dioxide, then into
Enter second level membrane module；The membrane component of the first order membrane module is ceramic filtration membrane, and the membrane component of the second level membrane module is
Composite nanometer filtering film；
S3: the waste lubricating oil after UF membrane is reacted under catalysts conditions, further sloughs waste lubricating oil by hydrofinishing
In the undesirable components such as all kinds of oxidation products and additive, through air lift and it is dry after obtain base oil and kerosene, the catalyst
For molybdenum-Raney nickel or super steady H-Y type molecular sieve-aluminium oxide.
2. waste lubricating oil environment protection regeneration method according to claim 1, which is characterized in that the composite nanometer filtering film is by such as
Lower step process preparation:
S1: preparing polyether sulfone basement membrane, polyether sulfone be dissolved in polyvinylpyrrolidone, configures the casting for being 30% containing mass fraction
Film liquid stirs 5-7h, and the standing and defoaming 2-3h in 45-50 DEG C of environment, by casting film after being cooled to room temperature under the conditions of 45-50 DEG C
Liquid is poured on knifing on glass, is put into film-forming in 10-25 DEG C of water-bath, impregnates 12- with deionized water after removing from glass plate
16h obtains polyether sulfone basement membrane, and is stored in spare in 10 DEG C of deionised waters；
S2: dispersing graphene oxide in deionized water, and the aqueous phase monomers solution that concentration is 1-15mg/L is made, and preparation is poly-
Ether sulfone basement membrane is immersed in 40-60 minutes in aqueous phase monomers solution and takes out, and the water phase list of polyether sulfone membrane surface is blotted with dryer
It is spare after liquid solution；
S3: n,N-Dimethylformamide is dissolved in acetylene, is configured the organic phase monomer solution of 1-5g/L, will be impregnated water phase list
The polyether sulfone basement membrane of liquid solution is immersed in organic phase monomer solution, and temperature is impregnates taking-up in 5 minutes at 20 DEG C, and in an oven 50
It is handled 10 minutes under the conditions of DEG C, obtains composite nanometer filtering film.
3. waste lubricating oil environment protection regeneration method according to claim 1, which is characterized in that the flocculant is polyaluminium
Aluminium stirs 2-4h at a temperature of 70 DEG C after flocculant is added into waste lubricating oil.
4. waste lubricating oil environment protection regeneration method according to claim 1, which is characterized in that the demulsifier is the demulsification of AR type
Agent stirs 1-3h after demulsifier is added into waste lubricating oil at 50 °C.
5. waste lubricating oil environment protection regeneration method according to claim 1, which is characterized in that the vacuum distillation condition is
100 DEG C, pressure is -0.5MPa.
6. waste lubricating oil environment protection regeneration method according to claim 1, which is characterized in that enter the first order membrane module
Pressure be 150MPa, temperature be 40-60 DEG C, stream of supercritical carbon dioxide speed be 10~20m/s, into the second level film group
The pressure of part is 0.6MPa, and temperature is 80-90 DEG C.
7. waste lubricating oil environment protection regeneration method according to claim 1, which is characterized in that the pressure of the hydrofinishing is
0.5-1.0MPa, temperature are 250-330 DEG C, hydrogen oil 800-1000, air speed 3-3.5h-1。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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