CN107855116B - Adsorbent for regeneration of semi-synthetic waste engine oil and use method thereof - Google Patents

Adsorbent for regeneration of semi-synthetic waste engine oil and use method thereof Download PDF

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CN107855116B
CN107855116B CN201711146407.5A CN201711146407A CN107855116B CN 107855116 B CN107855116 B CN 107855116B CN 201711146407 A CN201711146407 A CN 201711146407A CN 107855116 B CN107855116 B CN 107855116B
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CN107855116A (en
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瞿欢欢
朱至放
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Suzhou Bogen Bioseparation Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/261Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning
    • C10M175/0008Working-up used lubricants to recover useful products ; Cleaning with the use of adsorbentia
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning
    • C10M175/0058Working-up used lubricants to recover useful products ; Cleaning by filtration and centrifugation processes; apparatus therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46Materials comprising a mixture of inorganic and organic materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character

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Abstract

An adsorbent for regeneration of semi-synthetic used oil, comprising: 50-60 wt% of modified zeolite powder, 10-20 wt% of modified mesoporous silicon and 10-40 wt% of magnesium trisilicate; the using method comprises the following steps: the regenerated engine oil with better performance parameters is obtained by performing flocculation precipitation, acid washing, water washing and dehydration pretreatment on the waste engine oil, and then performing step-by-step adsorption and filtration by using the optimized organic bentonite, the optimized active carbon and the adsorbent of the invention; the adsorbent for regenerating semisynthetic waste engine oil has the characteristics of repeated use, high quality of produced regenerated engine oil and the like.

Description

Adsorbent for regeneration of semi-synthetic waste engine oil and use method thereof
Technical Field
The invention belongs to the field of motor vehicle lubricating oil, and particularly relates to an adsorbent for regenerating semisynthetic waste engine oil and a using method thereof.
Background
With the increasing quantity of motor vehicles in China, tens of thousands of tons of semi-synthetic waste engine oil are generated every year. If the used oil is directly discharged or treated by a simple incineration method, the environment can be seriously polluted. The existing mature technology is to crack the waste engine oil into light-chain gasoline which is then used as fuel, but the semi-synthetic engine oil is a high value-added product which is refined from petroleum and synthesized again, the production process consumes a large amount of resources, and the simple use of the semi-synthetic engine oil as fuel is also huge waste. With the development of economy and the shortage of petroleum resources, the supply and demand of semisynthetic engine oil are problematic, the price of the engine oil has greatly increased, the development of a waste engine oil regeneration technology has important significance for saving resources and protecting the environment, and meanwhile, good economic benefits can be generated.
The oil content of the absorbent such as activated carbon, activated clay and the like used in the existing waste engine oil regeneration method is high after absorption, the absorbent can not be reused after absorption, so that environmental pollution and cost are high, the oil content in the absorbed activated carbon and activated clay can reach 20-30% of the quality of the absorbent, the oil can cause pollution and waste if the absorbent is discarded, but the desorbed oil is turbid and has more impurities, and the quality of the oil product after secondary treatment is lower.
The existing method for regenerating the used oil by using the adsorbent generally has the following problems: 1. the regeneration period is longer, longer settling time is needed in the flocculation process, and the flocculation process is used for a plurality of times in the regeneration process of the waste engine oil, so that the regeneration period is prolonged. 2. The cost is higher, and the used raw materials are various and have larger consumption in the regeneration process of the waste engine oil, so that the cost required in the regeneration process of the waste engine oil is higher. 3. The regenerated quality is not high, the viscosity of the regenerated engine oil is greatly reduced, partial engine oil oxides are difficult to remove, and the regenerated engine oil can only be used as low-end engine oil after being mixed with new high-quality engine oil.
Disclosure of Invention
In view of the above-mentioned deficiencies in the prior art, the present invention provides an adsorbent for regeneration of semi-synthetic used oil, comprising: 50-60 wt% of modified zeolite powder, 10-20 wt% of modified mesoporous silicon and 10-40 wt% of magnesium trisilicate;
the preparation method of the modified zeolite comprises the following steps: mixing 30 parts of styrene, 30 parts of divinylbenzene, 10-20 parts of vinyl propionate and 5-10 parts of acrylamide at the temperature of 40-50 ℃ to obtain an oil phase mixture, adding the oil phase mixture into a reactor with a stirrer, a thermometer and a condensation reflux device, stirring at 500-min, adding 1-2 parts of benzoyl peroxide and 60 parts of 200 solvent oil into the oil phase mixture, stirring to fully dissolve the benzoyl peroxide and the 200 solvent oil, adding the obtained oil phase mixture into a water phase in stirring at the stirring speed of 500-600r/min, raising the temperature of a mixture system to 80-85 ℃ after the oil phase mixture forms uniform liquid drops in the water phase, carrying out suspension polymerization reaction for 16h, adding 400 parts of zeolite powder in the total amount of 300-min 3-4 times, after being uniformly mixed, the temperature is raised to 90-95 ℃ to be solidified for 12h, the mixture is cooled to normal temperature and then ground into powder by using a ball mill at low temperature, and the powder is sieved to obtain modified zeolite powder;
the preparation method of the modified mesoporous silicon comprises the following steps: 100 parts of deionized water 100mL and 1 part of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane are added into a metal reaction vessel with a stirrer, a thermometer and a condenser pipe, then 100 parts of mesoporous silicon 120 parts are slowly added under the stirring of 30-80r/min, and after reaction for 30 minutes at 30-40 ℃, filtration and drying are carried out, thus obtaining the silane modified mesoporous silicon.
Preferably, the adsorbent for regenerating semi-synthetic used oil, wherein: the fineness of the modified zeolite powder is more than 200 meshes.
A method for using the adsorbent for regeneration of semi-synthetic used oil according to claim 1, comprising the steps of:
(1) pretreatment of
Putting 100 parts of semi-synthetic waste engine oil into a plastic or ceramic container, adding 3-5 parts of alum and 2-3 parts of polysilicic acid flocculant, shaking and stirring for 30-50min, centrifuging for 3-5min at 4000-5000 r/min, and collecting upper oil to obtain first-stage upper clear oil; then adding 20-30 parts of 3-4mol/L sulfuric acid solution into the first-stage upper clear oil, placing the mixture in a constant temperature box at the set temperature of 55-60 ℃, shaking and stirring for 10-20min, keeping the temperature and standing for 10-12 hours, taking out the mixture for sealing, naturally settling for 1-2 days at room temperature, and collecting the upper oil to obtain second-stage upper clear oil; adding 0.1-0.2mol/L sodium hydroxide solution into the second-stage upper clear oil, washing the oil to be neutral, adding 20-30 parts of water for washing, shaking and stirring for 10-20min, centrifuging for 3-5min at 1000-2000 r/min, and collecting the upper oil to obtain third-stage upper clear oil; adding 20-30 parts of deionized water into the third-stage upper clear oil, washing with water, shaking and stirring for 10-20min, centrifuging at 1000-2000 r/min for 3-5min, and collecting the upper oil to obtain fourth-stage upper clear oil; adding 2-3 parts of anhydrous magnesium sulfate into the fourth-stage upper clear oil for dehydration, centrifuging for 3-5min at 4000-5000 r/min, and collecting the upper oil to obtain fifth-stage upper clear oil;
(2) adsorption filtration
Taking 90 parts of the upper clear oil of the fifth stage, putting the upper clear oil into a reaction kettle with a stirrer, adding 5-10 parts of organic bentonite under the conditions that the temperature is 110-120 ℃ and the speed is 200-300 r/min, carrying out primary adsorption for 50-60min, then stopping heating, blowing 10-15 ℃ of cold air to rapidly cool the oil, and cooling the oil to room temperature within 10-20 min; adding 3-5 parts of activated carbon while stirring while blowing cold air, standing and settling for 1-1.5 hours after cooling, completing preliminary adsorption, respectively collecting upper oil and lower sediment to obtain sixth-level upper oil and lower sediment, putting the sixth-level upper oil into a filter press for filtering, respectively collecting filtered clean oil and filter cakes to obtain first filtered clean oil and first filter cakes, putting the collected first filtered clean oil into a reaction kettle, adding 5-10 parts of an adsorbent for regenerating semisynthetic waste engine oil under the conditions of temperature of 10-20 ℃ and speed of 200-300 r/min for secondary adsorption for 35-60 minutes, standing and settling for 0.5-1.5 hours, and respectively collecting the upper oil and the lower sediment to obtain second filtered clean oil and second filter cakes; and (4) placing the second filtered clear oil into a high-speed centrifuge for centrifugation at 7000-8000 r/min for 3-5min to obtain the regenerated engine oil.
The lower layer adsorption sediment and the first and second filter cakes are carried with a large amount of oil, the lower layer adsorption sediment and the first and second filter cakes can be eluted by 1-2mol/L sodium hydroxide solution at 50-60 ℃, and the eluted oil is mixed with untreated waste engine oil for next treatment.
Preferably, the method for using the adsorbent for regenerating semisynthetic used oil comprises the following steps: the active carbon is coconut shell active carbon.
Preferably, the method for using the adsorbent for regenerating semisynthetic used oil comprises the following steps: the organic bentonite is calcium-based organic bentonite.
The regenerated engine oil can not be directly used as semisynthetic engine oil, can be mixed with mineral engine oil, is added with an engine oil additive, and can be used as semisynthetic engine oil or mineral engine oil.
The oil content in the second filter cake is less than 10%.
The invention has the beneficial effects that:
the invention provides an adsorbent for regenerating semisynthetic waste engine oil and a using method thereof, aiming at the defects of the conventional waste engine oil regeneration adsorbent, and the adsorbent has the characteristics of repeated use, high quality of produced regenerated engine oil and the like.
Detailed Description
The present invention will be described in further detail with reference to examples and comparative examples so that those skilled in the art can practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1
An adsorbent for regeneration of semi-synthetic used oil, comprising: 60 wt% of modified zeolite powder, 10 wt% of modified mesoporous silicon and 30 wt% of magnesium trisilicate; the modified zeolite powder has high surface area and good chemical stability, and the large-aperture resin coated on the surface of the modified zeolite powder has high adsorption capacity on macromolecular groups, nano carbon residue particles and the like in the semi-synthetic engine oil; the modified mesoporous silicon can effectively reduce the oil content of the adsorbent after adsorption, and has better functions of adsorbing oxidation products and denatured additives in engine oil; the modified zeolite powder and the modified mesoporous silicon still have good adsorption capacity after desorption treatment and can be repeatedly utilized, and the magnesium trisilicate can play a role in assisting adsorption, preventing the adsorbent from hardening and reducing the adsorption activity in use and storage
The preparation method of the modified zeolite comprises the following steps: mixing 30 parts of styrene, 30 parts of divinylbenzene, 20 parts of vinyl propionate and 5 parts of acrylamide at the temperature of 50 ℃ to obtain an oil phase mixture, adding the oil phase mixture into a reactor with a stirrer, a thermometer and a condensation reflux device, stirring at 500r/min, adding 1 part of benzoyl peroxide and 60 parts of 200 # solvent oil into the oil phase mixture, stirring to fully dissolve the benzoyl peroxide and the 200 # solvent oil, adding the obtained oil phase mixture into a stirring water phase, stirring at the speed of 500r/min to form uniform liquid drops of the oil phase mixture in the water phase, raising the temperature of a mixture system to 81 ℃, carrying out suspension polymerization reaction for 16 hours, adding 300 parts of zeolite powder in total in 3 times, uniformly mixing, raising the temperature to 90 ℃ to solidify for 12 hours, cooling the obtained mixture system to normal temperature, grinding the mixture system at low temperature by using a ball mill, sieving to obtain modified zeolite powder with fineness of more than 200 meshes; the zeolite powder is a zeolite filter material produced by Yusongsan water supply and drainage equipment factories in consolidated City.
The preparation method of the modified mesoporous silicon comprises the following steps: 100 parts of deionized water 100mL and 1 part of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane are added into a metal reaction vessel with a stirrer, a thermometer and a condenser pipe, then 120 parts of mesoporous silicon is slowly added under the stirring of 50r/min, the reaction is carried out for 30 minutes at the temperature of 40 ℃, and then the filtration and the drying are carried out, thus obtaining the silane modified mesoporous silicon. The mesoporous silicon is MCM-4 type mesoporous silicon produced by Shanghai Carbox phenanthrene biological medicine science and technology Limited.
A use method of an adsorbent for regenerating semisynthetic waste engine oil comprises the following steps:
(1) pretreatment of
Putting 100 parts of shell semisynthetic 5w-30 waste engine oil into a plastic container, adding 5 parts of alum and 3 parts of polysilicic acid flocculant (PSAA), shaking and stirring for 50min, pouring into a centrifuge, centrifuging for 5min at 5000r/min, and collecting upper oil to obtain first-stage upper clear oil; then adding 20 parts of 3mol/L sulfuric acid solution into the first-stage upper clear oil, placing the mixture in a constant temperature box, setting the temperature to be 60 ℃, shaking and stirring for 20min, keeping the temperature and standing for 12 hours, taking out the mixture, sealing the mixture, naturally settling the mixture at room temperature for 1 day, and collecting the upper oil to obtain second-stage upper clear oil; adding 0.2mol/L sodium hydroxide solution into the second-stage upper clear oil, washing the oil to be neutral, adding 30 parts of water for washing, shaking and stirring for 20min, centrifuging at 2000r/min for 3-5min, and collecting the upper oil to obtain third-stage upper clear oil; adding 30 parts of deionized water into the third-stage upper clear oil, washing with water, shaking and stirring for 20min, centrifuging at 2000r/min for 5min, and collecting upper oil to obtain fourth-stage upper clear oil; adding 3 parts of anhydrous magnesium sulfate into the fourth-stage upper clear oil for dehydration, centrifuging at 5000r/min for 5min, and collecting the upper oil to obtain fifth-stage upper clear oil; this step removes debris impurities in the oil, partially oxidized oil and byproducts of oil oxidation, partially degraded additives, and total moisture.
(2) Adsorption filtration
Taking 90 parts of the upper clear oil of the fifth level, putting the upper clear oil into a reaction kettle with a stirrer, adding 10 parts of calcium-based organic bentonite under the conditions that the temperature is 120 ℃ and the speed is 300r/min, carrying out preliminary adsorption for 60min, stopping heating, blowing cold air at 15 ℃ to rapidly cool the oil, and cooling the oil to room temperature within 15 min; adding 3 parts of activated carbon while stirring while blowing cold air, standing and settling for 1.5 hours after cooling is finished, finishing preliminary adsorption, respectively collecting upper-layer oil and lower-layer sediment to obtain sixth-level upper-layer oil and lower-layer adsorption sediment, putting the sixth-level upper-layer oil into a filter press for filtering, respectively collecting filtered clean oil and filter cakes to obtain first filtered clean oil and first filter cakes, putting the collected first filtered clean oil into a reaction kettle, adding 5 parts of adsorbent for regeneration of semi-synthetic waste engine oil under the conditions of temperature of 20 ℃ and speed of 300r/min for re-adsorption for 60min, then standing and settling for 1.5 hours, and respectively collecting the upper-layer oil and the lower-layer sediment to obtain second filtered clean oil and second filter cakes; and (4) placing the second filtered clear oil into a high-speed centrifuge for centrifugation for 5min at 8000r/min to obtain the regenerated engine oil.
This step removes most of the pigment remaining in the engine oil, nanoscale metal debris, residual carbon black particles, oxidized engine oil and its byproducts, and deactivated additives.
And a large amount of oil is carried in the lower-layer adsorption precipitate and the first and second filter cakes, the lower-layer adsorption precipitate and the first and second filter cakes are eluted by adopting 1mol/L sodium hydroxide solution at the temperature of 60 ℃, and the eluted oil is mixed with untreated waste engine oil to be treated together next time.
The activated carbon is coconut shell activated carbon with the fineness of 200 meshes.
Comparative example 1
A method for regenerating semi-synthetic waste engine oil comprises the following steps:
(1) pretreatment of
Putting 100 parts of shell semisynthetic 5w-30 waste engine oil into a plastic container, adding 3 parts of alum and 3 parts of polysilicic acid flocculant, shaking and stirring for 30min, centrifuging for 3min at 4000r/min, and collecting upper oil to obtain first-stage upper clear oil; then adding 20 parts of 3mol/L sulfuric acid solution into the first-stage upper layer clear oil, placing the mixture in a constant temperature box, setting the temperature to be 55 ℃, shaking and stirring for 10min, keeping the temperature and standing for 12 hours, taking out the mixture, sealing the mixture, naturally settling the mixture at room temperature for 1 day, and collecting the upper layer oil to obtain second-stage upper layer clear oil; adding 0.2mol/L sodium hydroxide solution into the second-stage upper clear oil, washing the oil to be neutral, adding 20 parts of water for washing, shaking and stirring for 10min, centrifuging at 2000r/min for 3min, and collecting the upper oil to obtain third-stage upper clear oil; adding 20 parts of deionized water into the third-stage upper clear oil, washing with water, shaking and stirring for 10min, centrifuging at 2000r/min for 3min, and collecting upper oil to obtain fourth-stage upper clear oil; adding 2 parts of anhydrous magnesium sulfate into the fourth-stage upper clear oil for dehydration, centrifuging at 4000r/min for 5min, and collecting the upper oil liquid to obtain fifth-stage upper clear oil;
(2) adsorption filtration
Taking 90 parts of the upper layer clear oil of the fifth stage, putting the upper layer clear oil into a reaction kettle with a stirrer, adding 5 parts of calcium-based organic bentonite under the conditions that the temperature is 110 ℃ and the speed is 300r/min, carrying out preliminary adsorption for 50min, stopping heating, blowing 10 ℃ cold air to rapidly cool the oil, and cooling the oil to room temperature within 15 min; adding 3 parts of coconut shell activated carbon with the fineness of 200 meshes while blowing cold air, standing and settling for 1h after cooling, completing preliminary adsorption, respectively collecting upper oil and lower sediment to obtain sixth-level upper oil and lower sediment, putting the sixth-level upper oil into a filter press for filtering, respectively collecting filtered clean oil and filter cakes to obtain first filtered clean oil and first filter cakes, putting the collected first filtered clean oil into a reaction kettle, adding 3 parts of coconut shell activated carbon and 5 parts of activated clay for secondary adsorption at the temperature of 100 ℃ and the speed of 200r/min for 60min, standing and settling for 1h, and respectively collecting the upper oil and the lower sediment to obtain second filtered clean oil and second filter cakes; and (4) putting the second filtered clear oil into a high-speed centrifuge for 3min at 7000r/min to obtain the regenerated engine oil.
Comparative example 2
On the basis of example 1, the modified zeolite powder and the modified mesoporous silicon were replaced with unmodified zeolite powder and unmodified mesoporous silicon to obtain a regenerated engine oil.
Comparative example 3
The regenerated engine oil obtained in example 1 and comparative examples 1 and 2 were tested by the corresponding methods, and the results were as follows:
example 1 regenerated engine oil performance data:
Figure BDA0001472567550000071
comparative example 1 regenerated oil performance data:
Figure BDA0001472567550000072
comparative example 2 regenerated oil performance data:
Figure BDA0001472567550000081
from the comparison, the regenerated engine oil obtained by adopting the adsorbent has better performance on main performance parameters.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.

Claims (10)

1. An adsorbent for regenerating semi-synthetic waste engine oil, which is characterized in that: the method comprises the following steps: 50-60 wt% of modified zeolite powder, 10-20 wt% of modified mesoporous silicon and 10-40 wt% of magnesium trisilicate;
the preparation method of the modified zeolite comprises the following steps: mixing 30 parts of styrene, 30 parts of divinylbenzene, 10-20 parts of vinyl propionate and 5-10 parts of acrylamide at the temperature of 40-50 ℃ to obtain an oil phase mixture, adding the oil phase mixture into a reactor with a stirrer, a thermometer and a condensation reflux device, stirring at the speed of 500r/min, adding 1-2 parts of benzoyl peroxide and 60 parts of 200 solvent oil into the oil phase mixture, stirring to fully dissolve the benzoyl peroxide and the 200 solvent oil, adding the obtained oil phase mixture into a water phase in stirring, stirring at the speed of 500r/min to 600r/min, raising the temperature of a mixture system to 80-85 ℃ after the oil phase mixture forms uniform liquid drops in the water phase, carrying out suspension polymerization reaction for 16h, adding 400 parts of zeolite powder in the total amount of 300-, after being uniformly mixed, the temperature is raised to 90-95 ℃ to be solidified for 12h, the mixture is cooled to normal temperature and then ground into powder by using a ball mill at low temperature, and the powder is sieved to obtain modified zeolite powder;
the preparation method of the modified mesoporous silicon comprises the following steps: 100 parts of deionized water 100mL and 1 part of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane are added into a metal reaction vessel with a stirrer, a thermometer and a condenser pipe, then 100 parts of mesoporous silicon 120 parts are slowly added under the stirring of 30-80r/min, and after reaction for 30 minutes at 30-40 ℃, filtration and drying are carried out, thus obtaining the silane modified mesoporous silicon.
2. The adsorbent for regeneration of semi-synthetic used oil according to claim 1, wherein: the fineness of the modified zeolite powder is more than 200 meshes.
3. A method of using the adsorbent for regeneration of semi-synthetic used oil according to claim 1, characterized in that: the method comprises the following steps:
(1) pretreatment of
Putting 100 parts of semi-synthetic waste engine oil into a plastic or ceramic container, adding 3-5 parts of alum and 2-3 parts of polysilicic acid flocculant, shaking and stirring for 30-50min, centrifuging for 3-5min at 4000-5000 r/min, and collecting upper oil to obtain first-stage upper clear oil; then adding 20-30 parts of 3-4mol/L sulfuric acid solution into the first-stage upper clear oil, placing the mixture in a constant temperature box at the set temperature of 55-60 ℃, shaking and stirring for 10-20min, keeping the temperature and standing for 10-12 hours, taking out the mixture for sealing, naturally settling for 1-2 days at room temperature, and collecting the upper oil to obtain second-stage upper clear oil; adding 0.1-0.2mol/L sodium hydroxide solution into the second-stage upper clear oil, washing the oil to be neutral, adding 20-30 parts of water for washing, shaking and stirring for 10-20min, centrifuging for 3-5min at 1000-2000 r/min, and collecting the upper oil to obtain third-stage upper clear oil; adding 20-30 parts of deionized water into the third-stage upper clear oil, washing with water, shaking and stirring for 10-20min, centrifuging at 1000-2000 r/min for 3-5min, and collecting the upper oil to obtain fourth-stage upper clear oil; adding 2-3 parts of anhydrous magnesium sulfate into the fourth-stage upper clear oil for dehydration, centrifuging for 3-5min at 4000-5000 r/min, and collecting the upper oil to obtain fifth-stage upper clear oil;
(2) adsorption filtration
Taking 90 parts of the upper clear oil of the fifth stage, putting the upper clear oil into a reaction kettle with a stirrer, adding 5-10 parts of organic bentonite under the conditions that the temperature is 110-120 ℃ and the speed is 200-300 r/min, carrying out primary adsorption for 50-60min, then stopping heating, blowing 10-15 ℃ of cold air to rapidly cool the oil, and cooling the oil to room temperature within 10-20 min; adding 3-5 parts of activated carbon while stirring while blowing cold air, standing and settling for 1-1.5 hours after cooling, completing preliminary adsorption, respectively collecting upper oil and lower sediment to obtain sixth-level upper oil and lower sediment, putting the sixth-level upper oil into a filter press for filtering, respectively collecting filtered clean oil and filter cakes to obtain first filtered clean oil and first filter cakes, putting the collected first filtered clean oil into a reaction kettle, adding 5-10 parts of an adsorbent for regenerating semisynthetic waste engine oil under the conditions of temperature of 10-20 ℃ and speed of 200-300 r/min for secondary adsorption for 35-60 minutes, standing and settling for 0.5-1.5 hours, and respectively collecting the upper oil and the lower sediment to obtain second filtered clean oil and second filter cakes; and (4) placing the second filtered clear oil into a high-speed centrifuge for centrifugation at 7000-8000 r/min for 3-5min to obtain the regenerated engine oil.
4. The use method of the adsorbent for regeneration of semi-synthetic used oil according to claim 3, wherein: and a large amount of oil is carried in the lower layer adsorption sediment and the first and second filter cakes.
5. The use method of the adsorbent for regeneration of semi-synthetic used oil according to claim 3, wherein: the lower layer adsorption precipitation and the first and second filter cakes can be eluted by 1-2mol/L sodium hydroxide solution at 50-60 ℃, and the eluted oil liquid is mixed with untreated waste engine oil for the next treatment.
6. The use method of the adsorbent for regeneration of semi-synthetic used oil according to claim 3, wherein: the active carbon is coconut shell active carbon.
7. The use method of the adsorbent for regeneration of semi-synthetic used oil according to claim 3, wherein: the organic bentonite is calcium-based organic bentonite.
8. The use method of the adsorbent for regeneration of semi-synthetic used oil according to claim 3, wherein: the regenerated engine oil cannot be directly used as a semi-synthetic engine oil.
9. The use method of the adsorbent for regeneration of semi-synthetic used oil according to claim 3, wherein: the regenerated engine oil is prepared with mineral engine oil, and is added with an engine oil additive to be used as semi-synthetic engine oil or mineral engine oil.
10. The use method of the adsorbent for regeneration of semi-synthetic used oil according to claim 3, wherein: the oil content in the second filter cake is less than 10%.
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