CN106824055A - A kind of sorbent regeneration process of waste lubricating oil - Google Patents
A kind of sorbent regeneration process of waste lubricating oil Download PDFInfo
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- CN106824055A CN106824055A CN201710059488.9A CN201710059488A CN106824055A CN 106824055 A CN106824055 A CN 106824055A CN 201710059488 A CN201710059488 A CN 201710059488A CN 106824055 A CN106824055 A CN 106824055A
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- Prior art keywords
- lubricating oil
- attapulgite
- waste lubricating
- acid
- washing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Treatment By Sorption (AREA)
- Lubricants (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention belongs to waste lubricant oil regeneration field, and in particular to a kind of sorbent regeneration process of waste lubricating oil, including:(1) after attapulgite is mixed with acid solution, ultrasonic washing is carried out, is then dried, obtain the attapulgite of acid treatment;(2) to addition distilled water and γ (methacryloxypropyl) propyl trimethoxy silicane, the 6h of stirring reaction 4 at 60 80 DEG C in the attapulgite of acid treatment;(3) washing and drying is carried out to product, is crushed, the attapulgite after being activated;(4) the standing sedimentation treatment at 25 80 DEG C by waste lubricating oil, then filters;(5) to the attapulgite put into the waste lubricating oil after filtering after the middle activation of step (4), the 8h of stirring and adsorbing 4 at 40 80 DEG C;(6) the waste lubricating oil standing sedimentation completed to absorption, is filtered, and filtrate is the lubricating oil of regeneration.The above method can effectively adsorb the heavy metal ion in waste lubricating oil, realize the effective regeneration of lubricating oil.
Description
Technical field
The invention belongs to waste lubricant oil regeneration field, and in particular to a kind of sorbent regeneration process of waste lubricating oil.
Background technology
Lubricating oil is commonly called as machine oil, is the maximum class material of main, consumption in lubricant, at home and abroad in lasting increasing
Trend long.Lubricating oil causes water phase components doping due to there is the effects such as oxidation, thermal decomposition, easily in use, together
When produce unsaturated hydrocarbons, the impurity such as heavy metal ion.Therefore, waste lubricating oil needs to change after being used for a while, but
Contain a large amount of base oils in waste lubricating oil, directly thrown aside or can cause the substantial amounts of wasting of resources as fuel combustion.Therefore,
How by the acid in waste lubricating oil, heavy metal ion, the removal of unsaturated hydrocarbons, make waste lubricant oil regeneration, as working as this life
The hot issue on boundary, all has great importance for environmental protection, lifting economic benefit and resource regeneration.
At present, the main Hydrofining Technology of method of external regeneration waste lubricating oil, one time input cost is higher, to reaction bar
Part requirement is also very strict.Domestic mainly to be regenerated using Emathlite method, low cost, technological process is simple.But treated
There is a problem of that yield is relatively low, regeneration efficiency is not high in journey.And this technique can produce substantial amounts of sour greasy filth, its post processing can be right
Environment causes serious burden, and bleaching earth adsorption agent to be difficult to regenerate, and causes the substantial amounts of wasting of resources.Therefore, it is badly in need of exploitation new
The method of adsorbent absorption regeneration waste lubricating oil.
The existing part researcher in the country develops new adsorbent for process for regeneration of waste lubricating oil, patent
CN104403776A discloses a kind of technique with amino functional silica based materials as adsorbent, by silica and oxygen
Amino is added in change aluminum, the acid in removal waste lubricating oil reaches waste lubricant oil regeneration purpose.Patent CN105617993A is public
Cloth is a kind of first saturation absorption waste lubricating oil adsorbent is separated with waste lubricating oil after, then adsorbent put into regenerated liquid, effectively
Realize adsorbent reactivation.Patent CN105505550A discloses a kind of with membrane separation technique retention larger molecular organicses and weight
The method of metal.But in current method, most of adsorbents are still smaller to the impurity absorption capacity in waste lubricating oil, regeneration
It is difficult, it is necessary to seek that adsorption capacity is high, separative efficiency adsorbent high.
The content of the invention
Invention broadly provides a kind of sorbent regeneration process of waste lubricating oil, in can effectively adsorbing waste lubricating oil
Heavy metal ion, realizes the effective regeneration of lubricating oil.Its technical scheme is as follows:A kind of sorbent regeneration process of waste lubricating oil, bag
Include following steps:
(1) after attapulgite is mixed with acid solution, ultrasonic washing is carried out, is then dried, obtain the attapulgite of acid treatment;
(2) to addition distilled water and γ-(methacryloxypropyl) propyl trimethoxy silicane in the attapulgite of acid treatment,
The stirring reaction 4-6h at 60-80 DEG C;
(3) washing and drying is carried out to product, is crushed, the attapulgite after being activated;
(4) the standing sedimentation treatment at 25-80 DEG C by waste lubricating oil, then filters;
(5) to the attapulgite put into the waste lubricating oil after filtering after the middle activation of step (4), stirred at 40-80 DEG C
Absorption 4-8h;
(6) to the waste lubricating oil standing sedimentation after the completion of absorption, then filtered, filtrate is the lubricating oil of regeneration.
Preferably, before the attapulgite mixes with acid, processed by high-temperature calcination, specific method is to take attapulgite
Original soil, crosses the treatment of 80-200 mesh sieves, then carries out high-temperature calcination at 550-650 DEG C.
Preferably, attapulgite and the mass ratio of acid solution are 1 in step (1):9-11, the acid solution is hydrochloric acid, salt
The concentration of acid is 4mol/L, and ultrasonic washing time is 20-40min, and the magnetic agitation of 380r/min is carried out in ultrasound washing.
Preferably, the addition of distilled water and γ-(methacryloxypropyl) propyl trimethoxy silicane is distinguished in step (2)
For the attapulgite of the acid treatment of 1-10g adds the distilled water of 1000ml and γ-(methacryloxypropyl) propyl group three of 2-10ml
Methoxy silane.
Preferably, product is washed respectively using absolute ethyl alcohol and deionized water in step (3), and side is washed
While carrying out 2000r/min centrifugations, after the completion of washing, dried at 110-130 DEG C.
Using the sorbent regeneration process of above-mentioned waste lubricating oil, the present invention has advantages below:
Attapulgite adsorption capacity after activation in the present invention is high, high to the impurity separative efficiency in waste lubricating oil, and
Adsorbent can be easily separated.And from accompanying drawing, it is therein heavy after processing waste lubricating oil using the inventive method activation attapulgite
Metal ion clearance is high, can facilitate economic recycling waste lubricating oil.
Brief description of the drawings
Fig. 1 be embodiment 1 in waste lubricating oil, through acid treatment attapulgite process after lubricating oil and after activated
Attapulgite treatment after Metals In Lubricating ion concentration figure.
Specific embodiment
Embodiment 1
Take after attapulgite original soil crosses 80 mesh sieves, be placed in crucible, be positioned in Muffle furnace, in 5h is calcined at 600 DEG C, take
Go out to cool down standby.According to solid-to-liquid ratio 1:10 hydrochloric acid for adding 4mol/L, ultrasonic 30min, at room temperature magnetic agitation 4h (380r/
Min), it is then centrifuged for, is washed with deionized water to without chlorion, is dried at 120 DEG C, it is standby after grinding sieving, obtain HCl treatment
Attapulgite.The attapulgite after 1000mL distilled water and the above-mentioned acid treatments of 2g is sequentially added in three-necked bottle, is stirred with back
Mix KH570, ultrasonic 30min that side adds 10mL;Then the stirring reaction 5h at 70 DEG C, product absolute ethyl alcohol and go from
Sub- water washing removes unnecessary KH570, and 2000r/min centrifugations dry, pulverize, the concave convex rod after being activated at 120 DEG C
Soil.After being filtered after waste lubricating oil is settled into 9h at 80 DEG C, the attapulgite after input activation, after stirring 6h at 80 DEG C, in
Filtered after 9h is settled at 80 DEG C, the lubricating oil for being regenerated.
Take HCl treatment in this case attapulgite and activation after attapulgite process waste lubricating oil respectively, determine without
The waste lubricating oil for the treatment of, through acid treatment attapulgite process lubricating oil and it is activated after attapulgite process lubricating oil
Middle metal ion content, as shown in Figure 1.As shown in Figure 1, after activated treatment attapulgite treatment Metals In Lubricating from
Sub- content is minimum, and all metal ions content is no more than the 0.3% of lubricating oil gross weight, it follows that the concave convex rod after activation
Soil is to the adsorption of metal ions efficiency high in waste lubricating oil.
Embodiment 2
Take after attapulgite original soil crosses 200 mesh sieves, be placed in crucible, be positioned in Muffle furnace, in calcining 7h at 650 DEG C,
Take out cooling standby.According to solid-to-liquid ratio 1:9 sulfuric acid for adding 4mol/L, ultrasonic 40min, at room temperature magnetic agitation 4h (380r/
Min), it is then centrifuged for, is washed with deionized water to sulfate radical-free ion, is dried at 110 DEG C, it is standby after grinding sieving, obtain at hydrochloric acid
The attapulgite of reason.The attapulgite after 1000mL distilled water and the above-mentioned acid treatments of 5g is sequentially added in three-necked bottle, then
The KH570, ultrasonic 35min of 10mL are added while stirring;Then the stirring reaction 5h at 80 DEG C, product absolute ethyl alcohol and
The unnecessary KH570 of deionized water washing removal, 2000r/min centrifugations dry, pulverize at 110 DEG C, concavo-convex after being activated
Rod soil.After being filtered after waste lubricating oil is settled into 10h at 70 DEG C, the attapulgite after input activation, after stirring 4h at 60 DEG C,
Filtered after 12h is settled at 80 DEG C, the lubricating oil for being regenerated.
Embodiment 3
Take after attapulgite original soil crosses 120 mesh sieves, be placed in crucible, be positioned in Muffle furnace, in calcining 5- at 550 DEG C
7h, takes out cooling standby.According to solid-to-liquid ratio 1:9 hydrochloric acid for adding 4mol/L, ultrasonic 20min, at room temperature magnetic agitation 4h
(380r/min), is then centrifuged for, and is washed with deionized water to without chlorion, is dried at 130 DEG C, standby after grinding sieving, obtains hydrochloric acid
The attapulgite for the treatment of.The attapulgite after 1000mL distilled water and the above-mentioned acid treatments of 10g is sequentially added in three-necked bottle, with
Add the KH570, ultrasonic 25min of 10mL while stirring afterwards;Then the stirring reaction 4h at 60 DEG C, product absolute ethyl alcohol
The KH570 unnecessary with deionized water washing removal, 2000r/min centrifugations dry, pulverize at 130 DEG C, recessed after being activated
Convex rod soil.After being filtered after waste lubricating oil is settled into 1h at 80 DEG C, the attapulgite after input activation stirs 4h at 60 DEG C
Afterwards, filtered after 5h is settled at 250 DEG C, the lubricating oil for being regenerated.
Embodiment 4
Take after attapulgite original soil crosses 150 mesh sieves, be placed in crucible, be positioned in Muffle furnace, in calcining 5h at 600 DEG C,
Take out cooling standby.According to solid-to-liquid ratio 1:10 hydrochloric acid for adding 4mol/L, ultrasonic 30min, at room temperature magnetic agitation 4h (380r/
Min), it is then centrifuged for, is washed with deionized water to without chlorion, is dried at 120 DEG C, it is standby after grinding sieving, obtain HCl treatment
Attapulgite.The attapulgite after 1000mL distilled water and the above-mentioned acid treatments of 1g is sequentially added in three-necked bottle, is stirred with back
Mix KH570, ultrasonic 25min that side adds 2mL;Then the stirring reaction 6h at 60 DEG C, product absolute ethyl alcohol and go from
Sub- water washing removes unnecessary KH570, and 2000r/min centrifugations dry, pulverize, the concave convex rod after being activated at 120 DEG C
Soil.After being filtered after waste lubricating oil is settled into 3h at 25 DEG C, the attapulgite after input activation, after stirring 6h at 80 DEG C, in
Filtered after 3h is settled at 25 DEG C, the lubricating oil for being regenerated.
Embodiment 5
Take after attapulgite original soil crosses 80 mesh sieves, be placed in crucible, be positioned in Muffle furnace, in 7h is calcined at 650 DEG C, take
Go out to cool down standby.According to solid-to-liquid ratio 1:10 sulfuric acid for adding 4mol/L, ultrasonic 20min, at room temperature magnetic agitation 4h (380r/
Min), it is then centrifuged for, is washed with deionized water to sulfate radical-free ion, is dried at 110 DEG C, it is standby after grinding sieving, obtain at hydrochloric acid
The attapulgite of reason.The attapulgite after 1000mL distilled water and the above-mentioned acid treatments of 4g is sequentially added in three-necked bottle, then
The KH570, ultrasonic 30min of 2mL are added while stirring;Then the stirring reaction 4h at 70 DEG C, product absolute ethyl alcohol and
The unnecessary KH570 of deionized water washing removal, 2000r/min centrifugations dry, pulverize at 120 DEG C, concavo-convex after being activated
Rod soil.After being filtered after waste lubricating oil is settled into 1h at 50 DEG C, the attapulgite after input activation, after stirring 6h at 80 DEG C,
Filtered after 1h is settled at 50 DEG C, the lubricating oil for being regenerated.
It will be apparent to those skilled in the art that technical scheme that can be as described above and design, make other various
It is corresponding to change and deformation, and all these change and deformation should all belong to the protection domain of the claims in the present invention
Within.
Claims (5)
1. a kind of sorbent regeneration process of waste lubricating oil, it is characterised in that:Comprise the following steps:
(1) after attapulgite is mixed with acid solution, ultrasonic washing is carried out, is then dried, obtain the attapulgite of acid treatment;
(2) to addition distilled water and γ-(methacryloxypropyl) propyl trimethoxy silicane in the attapulgite of acid treatment,
Stirring reaction 4-6h at 60-80 DEG C;
(3) washing and drying is carried out to product, is crushed, the attapulgite after being activated;
(4) the standing sedimentation treatment at 25-80 DEG C by waste lubricating oil, then filters;
(5) to the attapulgite put into the waste lubricating oil after filtering after the middle activation of step (4), the stirring and adsorbing at 40-80 DEG C
4-8h;
(6) to the waste lubricating oil standing sedimentation after the completion of absorption, then filtered, filtrate is the lubricating oil of regeneration.
2. the sorbent regeneration process of waste lubricating oil according to claim 1, it is characterised in that:The attapulgite is mixed with acid
Before conjunction, processed by high-temperature calcination, specific method is to take attapulgite original soil, cross the treatment of 80-200 mesh sieves, then 550-650
High-temperature calcination is carried out at DEG C.
3. the sorbent regeneration process of waste lubricating oil according to claim 1, it is characterised in that:Attapulgite in step (1)
It is 1 with the mass ratio of acid solution:9-11, the acid solution is hydrochloric acid, and the concentration of hydrochloric acid is 4mol/L, and ultrasonic washing time is
20-40min, the magnetic agitation of 380r/min is carried out in ultrasound washing.
4. the sorbent regeneration process of waste lubricating oil according to claim 1, it is characterised in that:In step (2) distilled water and
The attapulgite that the addition of γ-(methacryloxypropyl) propyl trimethoxy silicane is respectively the acid treatment of 1-10g is added
The distilled water of 1000ml and the γ of 2-10ml-(methacryloxypropyl) propyl trimethoxy silicane.
5. the sorbent regeneration process of waste lubricating oil according to claim 1, it is characterised in that:Using anhydrous in step (3)
Ethanol and deionized water are washed to product respectively, and carry out 2000r/min centrifugations in washing, after the completion of washing,
Dried at 110-130 DEG C.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110129123A (en) * | 2019-06-17 | 2019-08-16 | 天津清科环保科技有限公司 | A kind of regeneration method and its system of the emulsion containing heavy metal ion |
CN111659343A (en) * | 2020-06-16 | 2020-09-15 | 明光春计高分子材料有限公司 | Preparation method of attapulgite nanocomposite |
CN113603136A (en) * | 2021-08-25 | 2021-11-05 | 云南国钛金属股份有限公司 | Method for removing vanadium from titanium tetrachloride by using waste lubricating oil |
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CN110129123A (en) * | 2019-06-17 | 2019-08-16 | 天津清科环保科技有限公司 | A kind of regeneration method and its system of the emulsion containing heavy metal ion |
CN111659343A (en) * | 2020-06-16 | 2020-09-15 | 明光春计高分子材料有限公司 | Preparation method of attapulgite nanocomposite |
CN113603136A (en) * | 2021-08-25 | 2021-11-05 | 云南国钛金属股份有限公司 | Method for removing vanadium from titanium tetrachloride by using waste lubricating oil |
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Application publication date: 20170613 |