CN108913325A - The method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil - Google Patents
The method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil Download PDFInfo
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- CN108913325A CN108913325A CN201810558771.0A CN201810558771A CN108913325A CN 108913325 A CN108913325 A CN 108913325A CN 201810558771 A CN201810558771 A CN 201810558771A CN 108913325 A CN108913325 A CN 108913325A
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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
- C10M175/0008—Working-up used lubricants to recover useful products ; Cleaning with the use of adsorbentia
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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
- C10M175/005—Working-up used lubricants to recover useful products ; Cleaning using extraction processes; apparatus 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
- C10M175/0083—Lubricating greases
Abstract
The invention discloses a kind of methods of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil, and the waste lubricating oil loading container of processing to be regenerated is placed in thermostatic drying chamber and settles at least 12h, removes first upper layer edible vegetable oil；Then organic solvent is added in first upper layer edible vegetable oil and is stripped refinement treatment, obtained oil mixture is down to room temperature, after oil mixture is settled at least 2h again, remove secondary upper layer edible vegetable oil, secondary upper layer edible vegetable oil and composite metal oxide adsorbent is taken to carry out being mixed to form reactant system again, control reactant system temperature is 60~90 DEG C, carries out 20~40min of decoloration to secondary upper layer edible vegetable oil, it is finally separating and is removed metal composite oxide decolorising agent, obtains Reclaimed Base Oil.The present invention treated each quality index of waste oil reaches base oil requirement standard, whole process use anacidity alkali-free technique, and reclaimed oil high income, adsorbent high recycling rate, meet Green Sustainable requirement.
Description
Technical field
The present invention relates to a kind of methods of waste lubricating oil recycling and regeneration, more particularly to a kind of useless profit of solvent extraction
The method of lubricating oil recycling and regeneration further relates to one kind and recycles composite metal oxide adsorbent progress waste lubricating oil time
The method with regeneration is received, technical field of waste resourceful treatment is applied to.
Background technique
China national Bureau of Technical Supervision formulates《Waste lubricating oil recycling and regenerative use technology directive/guide》(GB/T17145--
1997) standard, it is specified that waste lubricating oil definition：" lubricating oil in various mechanical, equipment use processes, due to the oxygen by air
Change, thermal decomposition effect and impurity pollution, physicochemical property reach respective criteria for changing oil, and the oil changed is referred to as useless lubrication
Oil.Waste lubricating oil is difficult to degrade and remove in a natural environment, and itself there are also huge utility values, so being regenerated
Using not only conforming with the environmentally protective basic concept in China, moreover it is possible to bring great economic benefit.
The more commonly used technology of waste oil regenerating in China mainly has sedimentation-pickling-clay-filtered at present, distillation-solvent extraction-
Clay-filtered, pretreatment-distillation-furfural treatment-is clay-filtered, and carclazyte high temperature contact is without acid regeneration process etc..Sedimentation-pickling-
The characteristics of clay-filtered technique is that process flow is fairly simple, and required equipment and material price are cheap.But in operating process
Middle acid it is a large amount of using not only high risks can be carried out to the health care belt of operator, but also can cause environmental pollution.Carclazyte is high
Temperature contact is just that of avoiding in regenerative process without acid regeneration process and the characteristics of distillation-solvent extraction-clay-filtered technique to be had
The participation of acid, but the amount of the carclazyte due to adding in operating process is bigger, the yield of oil is relatively low.
Patent CN1162007A proposes a kind of method of waste oil regeneration carclazyte high temperature purification, and process flow includes that will give up
Oil, carclazyte, vapor three mix, and are heated to 300 DEG C, flash off moisture, light diesel fuel.It filters, is obtained again after being cooled to 130 DEG C
Oil generation.The method energy consumption is big, and is difficult to recycle after bleaching earth adsorption impurity, and new harm can be caused to environment.Patent
CN102746884A proposes a kind of method distilled including pretreatment-pickling-waste oil carclazyte, after this method settles pickling
Waste oil adds alkali neutralization to neutrality, when being heated to 100 DEG C, atlapulgite is added, stops stirring after stirring 20~30min, heating rises
Temperature；Start to be blown into vapor when waste oil temperature reaches 280~310 DEG C, maintains the temperature of waste oil to be no more than 320 DEG C, increase water
The amount of being blown into of vapor volume, until waste oil reaches expected viscosity and flash-point.Patent CN1539936A proposes one kind with alkane
Class solvent extraction replaces pickling and clay-filtered method, and alkane solvents are added at 30~130 DEG C of temperature in waste lubricating oil, are pressed
It is extracted under conditions of 3~16Mpa of power, extract liquor is sunk under conditions of 80~150 DEG C of temperature, 3~16Mpa of pressure
Extract liquor after sedimentation is sent into alkane solvents recovery tower under conditions of 90~250 DEG C of temperature, 2~12Mpa of pressure by drop
It is separated, isolates alkane solvents and lubricating oil component.The method needs scale effect, is not suitable for the national conditions in China,
And a large amount of organic solvent can be expended, cost is excessively high.
In conclusion mainly use carclazyte as adsorbent waste lubricating oil decoloration regeneration at present, though carclazyte has preferably
Adsorption effect, but there is a problem of that oil absorbency is excessively high；Purely being extracted using organic solvent can be such that cost increases significantly again；This at
For technical problem urgently to be resolved.
Summary of the invention
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
The method that solvent extraction combination composite metal oxide adsorbent regenerates waste lubricating oil is applied to waste lubricating oil decoloration process, entirely
Cheng Caiyong anacidity alkali-free technique, and reclaimed oil high income, adsorbent high recycling rate, meet Green Sustainable requirement.
The method of the present invention can eliminate the problems such as traditional sulfur process bring corrosion equipment, pollution environment, and simple process, operation
It is easy flexibly, low energy consumption, it is high-efficient, quality of reclaimed standard can be reached again.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil, by processing to be regenerated
Waste lubricating oil is packed into container, is placed in thermostatic drying chamber and settles at least 12h, removes first upper layer edible vegetable oil；Then on this is first
Organic solvent is added in layer edible vegetable oil and is stripped refinement treatment, the oil mixture obtained after extracting refinement treatment is down to
Room temperature, then by after oil mixture sedimentation at least 2h, secondary upper layer edible vegetable oil is removed, then take secondary upper layer edible vegetable oil and composition metal oxygen
Compound adsorbent carries out being mixed to form reactant system, and control reactant system temperature is 60~90 DEG C, to secondary upper layer edible vegetable oil
20~40min of decoloration is carried out, be finally separating and removes metal composite oxide decolorising agent, to obtain Reclaimed Base Oil.
As currently preferred technical solution, solvent extraction combination composite metal oxide adsorbent regenerates waste lubricating oil
Method, include the following steps：
A. by divalent calcium salt, trivalent iron salt and trivalent aluminium salt according to (10~12):1:The molar ratio of (3~5) is made into compound
Metal salt solution is 1 according to the molar ratio of trivalent iron salt and sodium hydroxide:The ratio of (32~100), by composition metal salting liquid
It is mixed with sodium hydroxide solution, and after 2~5h of stirring at normal temperature, carries out still aging 4~8h, it then will be mixed after ageing
It closes solution and is filtered washing, be dried at not higher than 105 DEG C, solid chemical compound obtained, then by solid chemical compound
2~3h of calcining is carried out at 500~800 DEG C, then the grinding of calcined product is broken to get metal composite oxide decoloration
Agent, it is spare as composite metal oxide adsorbent；The divalent calcium salt, trivalent iron salt and trivalent aluminium salt preferably use respectively
CaCl2Salt, FeCl3Salt and AlCl3Salt；
B. the waste lubricating oil of processing to be regenerated is packed into container, is placed in the thermostatic drying chamber not higher than 90 DEG C and settles at least
12h removes first upper layer edible vegetable oil, spare；
C. organic solvent will be added in the resulting first upper layer edible vegetable oil of the step b, and will be stripped refinement treatment, it is organic
The mass ratio of solvent and first upper layer edible vegetable oil is (4~6):1, the organic solvent is mixed by isopropanol and methyl ethyl ketone, is mixed
The volume ratio of isopropanol and methyl ethyl ketone is 3 in bonding solvent:(1~9)；
D. the oil mixture obtained after the step c is stripped refinement treatment is down to room temperature, then by oil-containing
Mixture settle at least 2h after, remove secondary upper layer edible vegetable oil, then take secondary upper layer edible vegetable oil with prepared in the step a it is compound
Metal oxide decolorising agent is mixed, and reactant system, secondary upper layer edible vegetable oil and metal composite oxide decolorising agent are formed
Mass ratio is (4~8):100, control reactant system temperature be 60~90 DEG C, to secondary upper layer edible vegetable oil carry out decoloration 20~
40min is finally separating and removes metal composite oxide decolorising agent, to obtain reclaimed oil.
As currently preferred technical solution, the waste lubricating oil of processing to be regenerated is useless gear oil, waste internal-combustion engine is oily, useless
Any one oily or any several miscella in hydraulic oil, waste heat Oil Guide.
As currently preferred technical solution, secondary upper layer edible vegetable oil is being taken to be mixed with metal composite oxide decolorising agent
It closes, when forming reactant system, metal composite oxide decolorising agent dosage is the 6~8% of secondary upper layer edible vegetable oil.
As currently preferred technical solution, to first upper layer edible vegetable oil and organic molten under the conditions of temperature is not higher than 60 DEG C
The mixture of agent is stirred, and is stripped refinement treatment.
As currently preferred technical solution, it will be finally separating and remove after decolourizing to secondary upper layer edible vegetable oil
Metal composite oxide decolorising agent collects the metal composite oxide decolorising agent after using, and after carrying out adsorbent activation processing, continues
It is used as metal composite oxide decolorising agent, metal composite oxide decolorising agent, which is recycled, can reuse 8~10 times.
As currently preferred technical solution, the metal composite oxide decolorising agent include calcium oxide, iron oxide and
Aluminium oxide.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage：
1. the method for the present invention is moistened using solvent extraction combination metal composite oxide regenerated for traditional handicraft
Lubricating oil, environmentally friendly, oil yield is high, and has the advantages that recycling；
2. the method for the present invention can eliminate the problems such as traditional sulfur process bring corrosion equipment, pollution environment, Er Qiegong
Skill is simple, convenient and flexible operation, low energy consumption, it is high-efficient, quality of reclaimed standard can be reached again；
3. the method for the present invention is finally separating to obtain Reclaimed Base Oil, treated, and each quality index of waste oil reaches base oil
It is required that standard；Whole process of the invention uses anacidity alkali-free technique, and reclaimed oil high income, adsorbent high recycling rate, meets green
Color sustainable development requirement.
Specific embodiment
Above scheme is described further below in conjunction with specific implementation example, the preferred embodiment of the present invention is described in detail such as
Under：
Embodiment one
In the present embodiment, a kind of method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil,
Include the following steps：
A. the anhydrous CaCl of 60mmol is weighed respectively2, 5mmol FeCl3·6H2The AlCl of O and 25mmol3·6H2O, it is molten
In 50mL without CO2The NaOH for being formulated as mixing salt solution in water, while weighing 160mmol is dissolved in 100mL deionized water and is configured to
Mixed ammonium/alkali solutions under magnetic agitation effects, mixing salt solution are slowly added into NaOH solution, is being stirred under normal temperature conditions
It mixes and carries out after 2h still aging, take out and filter after being aged 4h, be washed with water 2~3 times, obtain ternary metal in 105 DEG C of drying
Then hydroxide is calcined ternary metal hydroxide 3 hours at 750 DEG C, then calcined product is ground and is crushed, i.e.,
Metal composite oxide decolorising agent is obtained, it is spare as composite metal oxide adsorbent；
B. the useless gear oil of processing to be regenerated is packed into container, is placed in 90 DEG C of thermostatic drying chamber and settles 12h, removed big
Partial moisture, filters out large granular impurity, then removes first upper layer edible vegetable oil, spare；
C. organic solvent will be added in the resulting first upper layer edible vegetable oil of the step b, then is placed in the heating of constant temperature magnetic force and stirs
It mixes on device, opens heater switch and stirring switch, be warming up to 60 DEG C, control revolving speed, be stripped refinement treatment, complete constant temperature
After purification, stops heating and stirring, obtain oil mixture；The mass ratio for controlling organic solvent and first upper layer edible vegetable oil is 6:1,
The organic solvent is mixed by isopropanol and methyl ethyl ketone, and the volume ratio of in the mixed solvent isopropanol and methyl ethyl ketone is 3:1；
D. the oil mixture obtained after the step c is stripped refinement treatment is down to room temperature, by what is obtained
Oil mixture is transferred to separatory funnel, after settling 2h, removes secondary upper layer edible vegetable oil, then by secondary upper layer edible vegetable oil and in the step
The metal composite oxide decolorising agent prepared in rapid a is mixed, and reactant system is formed, and metal composite oxide decolorising agent is thrown
Dosage is the 6% of secondary upper layer edible vegetable oil, and control reactant system temperature is 80 DEG C, carries out decoloration 20min to secondary upper layer edible vegetable oil,
It is finally separating and removes metal composite oxide decolorising agent, to obtain the lubricating oil of clear pale yellow color.
Experimental test and analysis：
Percent of decolourization test and rate of recovery test are carried out to the regenerated waste lubricating oil of the present embodiment, test result is as shown in table 1.
Embodiment two
The present embodiment is basically the same as the first embodiment, and is particular in that：
In the present embodiment, a kind of method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil,
Include the following steps：
A. the anhydrous CaCl of 60mmol is weighed respectively2, 5mmol FeCl3·6H2The AlCl of O and 25mmol3·6H2O, it is molten
In 50mL without CO2The NaOH for being formulated as mixing salt solution in water, while weighing 160mmol is dissolved in 100mL deionized water and is configured to
Mixed ammonium/alkali solutions under magnetic agitation effects, mixing salt solution are slowly added into NaOH solution, is being stirred under normal temperature conditions
It mixes and carries out after 5h still aging, take out and filter after being aged 4h, be washed with water 2~3 times, obtain ternary metal in 105 DEG C of drying
Then hydroxide is calcined ternary metal hydroxide 3 hours at 750 DEG C, then calcined product is ground and is crushed, i.e.,
Metal composite oxide decolorising agent is obtained, it is spare as composite metal oxide adsorbent；
B. the useless gear oil of processing to be regenerated is packed into container, is placed in 90 DEG C of thermostatic drying chamber and settles 12h, removed big
Partial moisture, filters out large granular impurity, then removes first upper layer edible vegetable oil, spare；
C. organic solvent will be added in the resulting first upper layer edible vegetable oil of the step b, then is placed in the heating of constant temperature magnetic force and stirs
It mixes on device, opens heater switch and stirring switch, be warming up to 60 DEG C, control revolving speed, be stripped refinement treatment, complete constant temperature
After purification, stops heating and stirring, obtain oil mixture；The mass ratio for controlling organic solvent and first upper layer edible vegetable oil is 6:1,
The organic solvent is mixed by isopropanol and methyl ethyl ketone, and the volume ratio of in the mixed solvent isopropanol and methyl ethyl ketone is 1:1；
D. the oil mixture obtained after the step c is stripped refinement treatment is down to room temperature, by what is obtained
Oil mixture is transferred to separatory funnel, after settling 2h, removes secondary upper layer edible vegetable oil, then by secondary upper layer edible vegetable oil and in the step
The metal composite oxide decolorising agent prepared in rapid a is mixed, and reactant system is formed, and metal composite oxide decolorising agent is thrown
Dosage is the 6% of secondary upper layer edible vegetable oil, and control reactant system temperature is 80 DEG C, carries out decoloration 20min to secondary upper layer edible vegetable oil,
It is finally separating and removes metal composite oxide decolorising agent, to obtain the lubricating oil of clear pale yellow color.
Experimental test and analysis：
Percent of decolourization test and rate of recovery test are carried out to the regenerated waste lubricating oil of the present embodiment, test result is as shown in table 1.
Embodiment three
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, a kind of method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil,
Include the following steps：
A. the anhydrous CaCl of 60mmol is weighed respectively2, 5mmol FeCl3·6H2The AlCl of O and 25mmol3·6H2O, it is molten
In 50mL without CO2The NaOH for being formulated as mixing salt solution in water, while weighing 160mmol is dissolved in 100mL deionized water and is configured to
Mixed ammonium/alkali solutions under magnetic agitation effects, mixing salt solution are slowly added into NaOH solution, is being stirred under normal temperature conditions
It mixes and carries out after 4h still aging, take out and filter after being aged 4h, be washed with water 2~3 times, obtain ternary metal in 105 DEG C of drying
Then hydroxide is calcined ternary metal hydroxide 3 hours at 750 DEG C, then calcined product is ground and is crushed, i.e.,
Metal composite oxide decolorising agent is obtained, it is spare as composite metal oxide adsorbent；
B. the useless gear oil of processing to be regenerated is packed into container, is placed in 90 DEG C of thermostatic drying chamber and settles 12h, removed big
Partial moisture, filters out large granular impurity, then removes first upper layer edible vegetable oil, spare；
C. organic solvent will be added in the resulting first upper layer edible vegetable oil of the step b, then is placed in the heating of constant temperature magnetic force and stirs
It mixes on device, opens heater switch and stirring switch, be warming up to 60 DEG C, control revolving speed, be stripped refinement treatment, complete constant temperature
After purification, stops heating and stirring, obtain oil mixture；The mass ratio for controlling organic solvent and first upper layer edible vegetable oil is 6:1,
The organic solvent is mixed by isopropanol and methyl ethyl ketone, and the volume ratio of in the mixed solvent isopropanol and methyl ethyl ketone is 1:3；
D. the oil mixture obtained after the step c is stripped refinement treatment is down to room temperature, by what is obtained
Oil mixture is transferred to separatory funnel, after settling 2h, removes secondary upper layer edible vegetable oil, then by secondary upper layer edible vegetable oil and in the step
The metal composite oxide decolorising agent prepared in rapid a is mixed, and reactant system is formed, and metal composite oxide decolorising agent is thrown
Dosage is the 6% of secondary upper layer edible vegetable oil, and control reactant system temperature is 80 DEG C, carries out decoloration 20min to secondary upper layer edible vegetable oil,
It is finally separating and removes metal composite oxide decolorising agent, to obtain the lubricating oil of clear pale yellow color.
Experimental test and analysis：
Percent of decolourization test and rate of recovery test are carried out to the regenerated waste lubricating oil of the present embodiment, test result is as shown in table 1.
Example IV
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, a kind of method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil,
Include the following steps：
A. the anhydrous CaCl of 50mmol is weighed respectively2, 5mmol FeCl3·6H2The AlCl of O and 15mmol3·6H2O, it is molten
In 50mL without CO2The NaOH for being formulated as mixing salt solution in water, while weighing 500mmol is dissolved in 100mL deionized water and is configured to
Mixed ammonium/alkali solutions under magnetic agitation effects, mixing salt solution are slowly added into NaOH solution, is being stirred under normal temperature conditions
It is carried out after mixing 4h, takes out and filter after being aged 8h, be washed with water 2~3 times, obtain ternary metal hydroxide in 105 DEG C of drying,
Then ternary metal hydroxide is calcined 2 hours at 800 DEG C, then the grinding of calcined product is broken to get compound gold
Belong to oxide decolorising agent, it is spare as composite metal oxide adsorbent；
B. the useless gear oil of processing to be regenerated is packed into container, is placed in 90 DEG C of thermostatic drying chamber and settles 12h, removed big
Partial moisture, filters out large granular impurity, then removes first upper layer edible vegetable oil, spare；
C. organic solvent will be added in the resulting first upper layer edible vegetable oil of the step b, then is placed in the heating of constant temperature magnetic force and stirs
It mixes on device, opens heater switch and stirring switch, be warming up to 60 DEG C, control revolving speed, be stripped refinement treatment, complete constant temperature
After purification, stops heating and stirring, obtain oil mixture；The mass ratio for controlling organic solvent and first upper layer edible vegetable oil is 4:1,
The organic solvent is mixed by isopropanol and methyl ethyl ketone, and the volume ratio of in the mixed solvent isopropanol and methyl ethyl ketone is 1:1；
D. the oil mixture obtained after the step c is stripped refinement treatment is down to room temperature, by what is obtained
Oil mixture is transferred to separatory funnel, after settling 2h, removes secondary upper layer edible vegetable oil, then by secondary upper layer edible vegetable oil and in the step
The metal composite oxide decolorising agent prepared in rapid a is mixed, and reactant system is formed, and metal composite oxide decolorising agent is thrown
Dosage is the 8% of secondary upper layer edible vegetable oil, and control reactant system temperature is 90 DEG C, carries out decoloration 40min to secondary upper layer edible vegetable oil,
It is finally separating and removes metal composite oxide decolorising agent, to obtain the lubricating oil of clear pale yellow color.
Experimental test and analysis：
Percent of decolourization test and rate of recovery test are carried out to the regenerated waste lubricating oil of the present embodiment, test result is as shown in table 1.
Embodiment five
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, a kind of method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil,
Include the following steps：
A. the anhydrous CaCl of 50mmol is weighed respectively2, 5mmol FeCl3·6H2The AlCl of O and 15mmol3·6H2O, it is molten
In 50mL without CO2The NaOH for being formulated as mixing salt solution in water, while weighing 500mmol is dissolved in 100mL deionized water and is configured to
Mixed ammonium/alkali solutions under magnetic agitation effects, mixing salt solution are slowly added into NaOH solution, is being stirred under normal temperature conditions
It is carried out after mixing 4h, takes out and filter after being aged 8h, be washed with water 2~3 times, obtain ternary metal hydroxide in 105 DEG C of drying,
Then ternary metal hydroxide is calcined 2 hours at 500 DEG C, then the grinding of calcined product is broken to get compound gold
Belong to oxide decolorising agent, it is spare as composite metal oxide adsorbent；
B. the useless gear oil of processing to be regenerated is packed into container, is placed in 90 DEG C of thermostatic drying chamber and settles 12h, removed big
Partial moisture, filters out large granular impurity, then removes first upper layer edible vegetable oil, spare；
C. organic solvent will be added in the resulting first upper layer edible vegetable oil of the step b, then is placed in the heating of constant temperature magnetic force and stirs
It mixes on device, opens heater switch and stirring switch, be warming up to 60 DEG C, control revolving speed, be stripped refinement treatment, complete constant temperature
After purification, stops heating and stirring, obtain oil mixture；The mass ratio for controlling organic solvent and first upper layer edible vegetable oil is 4:1,
The organic solvent is mixed by isopropanol and methyl ethyl ketone, and the volume ratio of in the mixed solvent isopropanol and methyl ethyl ketone is 1:1；
D. the oil mixture obtained after the step c is stripped refinement treatment is down to room temperature, by what is obtained
Oil mixture is transferred to separatory funnel, after settling 2h, removes secondary upper layer edible vegetable oil, then by secondary upper layer edible vegetable oil and in the step
The metal composite oxide decolorising agent prepared in rapid a is mixed, and reactant system is formed, and metal composite oxide decolorising agent is thrown
Dosage is the 4% of secondary upper layer edible vegetable oil, and control reactant system temperature is 60 DEG C, carries out decoloration 30min to secondary upper layer edible vegetable oil,
It is finally separating and removes metal composite oxide decolorising agent, to obtain the lubricating oil of clear pale yellow color.
Experimental test and analysis：
Percent of decolourization test and rate of recovery test are carried out to the regenerated waste lubricating oil of the present embodiment, test result is as shown in table 1.
Analysis test is carried out to regenerated waste lubricating oil prepared in the above embodiments and evaluation is as follows：
Evaluation method：
1. percent of decolourization is tested：
Percent of decolourization is calculated using the absorbance before and after spectrophotometric determination lubrication oil decolorization.Calculation formula is percent of decolourization
(%)=(A0-A1)/A0× 100%, wherein A0For the absorbance before decolorization, A1For the absorbance after decolorization.
2. the rate of recovery is tested：
The quality of decolorization front and back lubricating oil is weighed to calculate the rate of recovery.Calculation formula is the rate of recovery (%)=(M0-
M1)/M0× 100%, wherein M0For the quality before decolorization, M1For the quality after decolorization.
1. one~embodiment of the embodiment of the present invention five of table prepares waste lubricating oil and carries out percent of decolourization test and rate of recovery test in fact
Test result
| Percent of decolourization (%) | The rate of recovery (%) | |
| Embodiment one | 90.25 | 92.55 |
| Embodiment two | 92.35 | 92.05 |
| Embodiment three | 91.01 | 90.30 |
| Example IV | 90.06 | 92.70 |
| Embodiment five | 87.95 | 93.10 |
The method that the above embodiment of the present invention solvent extraction combination metal composite oxide regenerates waste lubricating oil, will be to be regenerated
Waste lubricating oil be packed into container, be placed in sedimentation in thermostatic drying chamber, take first upper layer edible vegetable oil；It is added in the first upper layer edible vegetable oil
Organic solvent is stripped purification, when the mass ratio of organic solvent and first upper layer edible vegetable oil is 6:1, the body of isopropanol and methyl ethyl ketone
Product is than being 1:When 1, extracting refining effect is best.Mixture after extracting purification is down to room temperature, then takes secondary upper layer edible vegetable oil
It is mixed with metal composite oxide decolorising agent, works as Ca:Fe:Al=12:1:When 5, adsorbent decolorizing effect and stability are preferable,
Then control temperature of reaction system decolourizes, and is finally separating to obtain Reclaimed Base Oil, treated, and each quality index of waste oil is equal
Reach base oil requirement standard.The above embodiment of the present invention is lubricated using solvent extraction combination metal composite oxide regenerated
Oil, environmentally friendly, oil yield is high, and has the advantages that recycling；The method of the present invention can eliminate traditional sulfuric acid work
Skill bring corrode equipment, pollution environment the problems such as, and simple process, convenient and flexible operation, low energy consumption, it is high-efficient, again energy
Reach quality of reclaimed standard；The method of the present invention is finally separating to obtain Reclaimed Base Oil, and treated, and each quality index of waste oil is equal
Reach base oil requirement standard；Whole process of the invention uses anacidity alkali-free technique, and reclaimed oil high income, adsorbent recycling rate of waterused
Height meets Green Sustainable requirement.
Embodiment six
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, it will be finally separating after decolourizing to secondary upper layer edible vegetable oil and remove composition metal oxidation
Object decolorising agent collects the metal composite oxide decolorising agent after using, and after carrying out adsorbent activation processing, continues as composition metal
Oxide decolorising agent uses, and metal composite oxide decolorising agent, which is recycled, can reuse 8~10 times.The present embodiment circulation benefit
Waste lubricating oil recycling and regeneration are carried out with composite metal oxide adsorbent, reduces the processing cost of regeneration waste lubricating oil,
It is of great significance to waste resource recovery processing.
The embodiment of the present invention is illustrated above, but the present invention is not limited to the above embodiments, it can also be according to this hair
The purpose of bright innovation and creation makes a variety of variations, and that does under the Spirit Essence and principle of all technical solutions according to the present invention changes
Become, modification, substitution, combination or simplified, should be equivalent substitute mode, as long as meeting goal of the invention of the invention, as long as not
Away from the technical principle and invention of the method for solvent extraction combination composite metal oxide adsorbent of the present invention regeneration waste lubricating oil
Design, belongs to protection scope of the present invention.
Claims (8)
1. a kind of method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil, it is characterised in that：It will be to
The waste lubricating oil of regeneration treatment is packed into container, is placed in thermostatic drying chamber and settles at least 12h, removes first upper layer edible vegetable oil；Then
Organic solvent is added in the first upper layer edible vegetable oil and is stripped refinement treatment, the oil-containing that will be obtained after extracting refinement treatment
Mixture is down to room temperature, then after oil mixture is settled at least 2h, removes secondary upper layer edible vegetable oil, then take secondary upper layer edible vegetable oil with
Composite metal oxide adsorbent carries out being mixed to form reactant system, and control reactant system temperature is 60~90 DEG C, to two
Secondary upper layer edible vegetable oil carries out 20~40min of decoloration, is finally separating and removes metal composite oxide decolorising agent, to obtain regeneration base
Plinth oil.
2. the method for solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil according to claim 1,
It is characterized in that, includes the following steps：
A. by divalent calcium salt, trivalent iron salt and trivalent aluminium salt according to (10~12):1:The molar ratio of (3~5) is made into composition metal
Salting liquid is 1 according to the molar ratio of trivalent iron salt and sodium hydroxide:The ratio of (32~100), by composition metal salting liquid and hydrogen
Sodium hydroxide solution is mixed, and after 2~5h of stirring at normal temperature, is then allowed to stand 4~8h of ageing, then that the mixing after ageing is molten
Liquid is filtered washing, is dried at not higher than 105 DEG C, solid chemical compound is obtained, then by solid chemical compound 500
Carry out 2~3h of calcining at~800 DEG C, then the grinding of calcined product is broken to get metal composite oxide decolorising agent, as
Composite metal oxide adsorbent is spare；
B. the waste lubricating oil of processing to be regenerated is packed into container, is placed in the thermostatic drying chamber not higher than 90 DEG C and settles at least 12h,
First upper layer edible vegetable oil is removed, it is spare；
C. organic solvent will be added in the resulting first upper layer edible vegetable oil of the step b, and will be stripped refinement treatment, organic solvent
Mass ratio with first upper layer edible vegetable oil is (4~6):1, the organic solvent is mixed by isopropanol and methyl ethyl ketone, is mixed molten
The volume ratio of isopropanol and methyl ethyl ketone is 3 in agent:(1~9)；
D. the oil mixture obtained after the step c is stripped refinement treatment is down to room temperature, then oil-containing is mixed
After object settles at least 2h, secondary upper layer edible vegetable oil is removed, then the composition metal for taking secondary upper layer edible vegetable oil and preparing in the step a
Oxide decolorising agent is mixed, and reactant system, the quality of secondary upper layer edible vegetable oil and metal composite oxide decolorising agent are formed
Than for (4~8):100, control reactant system temperature is 60~90 DEG C, carries out 20~40min of decoloration to secondary upper layer edible vegetable oil,
It is finally separating and removes metal composite oxide decolorising agent, to obtain reclaimed oil.
3. the method for solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil according to claim 1 or claim 2,
It is characterized in that：The waste lubricating oil of processing to be regenerated is useless gear oil, waste internal-combustion engine oil, waste hydraulic oil, times in waste heat Oil Guide
It anticipates a kind of oily or any several miscella.
4. the method for solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil according to claim 1 or claim 2,
It is characterized in that：Secondary upper layer edible vegetable oil is being taken to be mixed with metal composite oxide decolorising agent, it is multiple when forming reactant system
Close 6~8% that metal oxide decolorising agent dosage is secondary upper layer edible vegetable oil.
5. the method for solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil according to claim 1 or claim 2,
It is characterized in that：The mixture of first upper layer edible vegetable oil and organic solvent is stirred under the conditions of temperature is not higher than 60 DEG C, into
Row extracting refinement treatment.
6. the method for solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil according to claim 1 or claim 2,
It is characterized in that：It will be finally separating and be removed metal composite oxide decolorising agent after decolourizing to secondary upper layer edible vegetable oil, receive
Metal composite oxide decolorising agent after collection use after carrying out adsorbent activation processing, continues to decolourize as metal composite oxide
Agent uses, and metal composite oxide decolorising agent, which is recycled, can reuse 8~10 times.
7. the method for solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil according to claim 1 or claim 2,
It is characterized in that：The metal composite oxide decolorising agent includes calcium oxide, iron oxide and aluminium oxide.
8. the method for solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil according to claim 2,
It is characterized in that：In the step a, the divalent calcium salt, trivalent iron salt and trivalent aluminium salt are respectively CaCl2Salt, FeCl3Salt and
AlCl3Salt.
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