CN103881800B - A kind of pretreated method of waste lubricating oil - Google Patents
A kind of pretreated method of waste lubricating oil Download PDFInfo
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- CN103881800B CN103881800B CN201410105091.5A CN201410105091A CN103881800B CN 103881800 B CN103881800 B CN 103881800B CN 201410105091 A CN201410105091 A CN 201410105091A CN 103881800 B CN103881800 B CN 103881800B
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Abstract
Provided by the invention is a kind of pretreated method of waste lubricating oil, comprises the following steps: waste lubricating oil is carried out sedimentation, drying, obtains oil mixture A; Described oil mixture A organic solvent carrying out flocculation refining, obtain oil mixture B, described organic solvent refers to hydroxyethylethylene diamine; Described oil mixture B is carried out constant temperature sedimentation, separation, obtains pre-treatment oil. The present invention can remove colloid, bituminous matter, sulfide, oxide compound, metal and unsaturated hydrocarbons etc. well, obtain limpid bright pre-treatment oil, and method is simple, easy and safe to operate, reclaim equiment drops into low, the national conditions that waste oil regeneration factory of applicable China small scale, fund are few, backward in technique, the waste residue that flocculation process produces simultaneously is available after carrying out reprocessing makes ink, good economic benefit can be produced, and reduce secondary pollution.
Description
Technical field
The present invention relates to technical field of lubricating oil, in particular to a kind of pretreated method of waste lubricating oil.
Background technology
Lubricating oil is for all kinds of mechanically to reduce friction, protection machinery and the liquid lubricant of workpiece, mainly plays antifriction, cooling, sealing, buffering, the effect such as antirust and cleaning. Use in the environment such as high temperature, high pressure owing to lubricating oil is many, after using for some time, due to physics or chemical factor, generate such as impurity such as aldehyde, ketone, resin, pitch colloidal materials, carbon black and organic acid, salt, water, metal fragments, the performance of lubricating oil is caused to change, can not continue again to use, be replaced, just become waste lubricating oil. Waste lubricating oil not only exists various oxidation products (mainly carboxylic-acid, carboxylic acid esters, aldehyde class, ketone class, alcohol class, superoxide etc.), also containing undesirable components such as moisture, metal particle, carbon granule, dust, greasy filth, additive, residue pitch and mechanical impuritys, these undesirable components can seriously affect waste oil and re-refine each link of following process, such as hydrofining, distillation, membrane separation technique etc. When waste oil carries out hydrofining and hydrocracking, soot, additive and resolvent thereof in waste oil, and metal all can be deposited on catalyst surface, causes catalyst deactivation; After thermal processes act when waste oil distills destroys detergent-dispersant additive, these solid impurities suspended will be deposited on column plate, filler and boiler tube, and blocking channel, affects the operation of distillation plant; When waste oil uses membrane separation technique to regenerate, membrane pores is very easily polluted by these undesirable components or is blocked, and affects separating effect. The pre-treatment of waste oil is almost the first step of all waste oil regenerations, is also a crucial step. But industrial mostly only with simple sedimentation, filtration, as the preprocessing process that waste oil is refining, far do not reach the effect of expection.
A kind of waste lubricating oil pretreatment process that patent CN103045342A announces, comprises the following steps: waste oil is filtered by (1), de-except great machinery impurity; (2) add quaternary ammonium salt organic floculant and the phosphoric acid salt metal remover of 0.5��3.0%, constant at 30 DEG C stirring reaction 20��60min; (3) reaction product is carried out atmospheric flashing, with de-except lighter hydrocarbons, moisture and gasoline; (4) centrifugal de-slag, obtains pre-treatment oil.
Patent CN201470164U discloses a kind of energy saving and environment friendly waste oil pre-processing setting tank, comprises waste oil storage tank, storage tank supporting structure, blowdown interface, waste gas purification apparatus, and it has concurrently and stores waste oil and solid substance precipitation, pretreated effect of dewatering. The process existed can be solved in current waste oil preprocessing process and go out the problems such as oil production sex change, water ratio height, solid content height.
Patent CN101880588A discloses the recovery pretreatment process of a kind of waste machine oil, described method comprises the following steps: add glassed steel reaction vessels by leaving standstill the waste oil after anhydrating, under agitation it is heated to 94��98 DEG C, then slowly drip in 15min and add 70��aqueous sulfuric acid (volume ratio of aqueous sulfuric acid and waste oil is 1:200) of 75% volume ratio, drip and continue maintenance 94��98 DEG C, 45��60min after adding end, stop stirring, leave standstill 60��90min again, remove the moisture after layering, finally take advantage of waste heat filter can obtain limpid oily without water pretreatment.
At present, though the pretreatment unit of waste oil and pretreatment process are substantially feasible, but still there is following problem: (1) needs to add soda acid, both etching apparatus, again contaminate environment; (2) process is complicated, the time is long; (3) cost is higher; (4) pre-treatment oil quality is poor.
Summary of the invention
It is an object of the invention to overcome the shortcoming of above-mentioned waste lubricating oil pretreatment process, there is provided one can remove the undesirable components such as overwhelming majority moisture, mechanical impurity, additive, residue and metal, the waste lubricating oil being applicable to all kinds, the trade mark, and there is the waste lubricating oil pretreatment process of the features such as renovation process is simple, easy and safe to operate, reclaim equiment input is low.
For achieving the above object, the present invention provides following technical scheme:
A kind of pretreated method of waste lubricating oil, comprises the following steps:
1. waste lubricating oil is carried out sedimentation, drying, obtain oil mixture A;
2. described oil mixture A organic solvent carrying out flocculation refining, obtain oil mixture B, described organic solvent refers to hydroxyethylethylene diamine;
3. described oil mixture B is carried out constant temperature sedimentation, separation, obtain pre-treatment oil.
Further, the mass ratio of described solvent and described oil mixture A is 1��15:100;
Further, described refining temperature 50��80 DEG C;
Further, the described refining time is 30��90min;
Further, the temperature of described constant temperature sedimentation is 50��80 DEG C;
Further, the time of described constant temperature sedimentation is 2��7h.
The useful effect of the present invention is:
Every condition requirement of present invention flocculation agent, carry out a large amount of screening operations, finally have chosen the pretreating agent of hydroxyethylethylene diamine as waste lubricating oil, and hydroxyethylethylene diamine is simultaneously containing amido, the straight-chain molecule of hydroxyl structure, due to the sucking action of Sauerstoffatom in impurity particle, make hydroxyl, hydrogen atom in amino is lively and forms hydrogen bond, realize bridging action, hydroxyl in the oxy radical of impurity particle surface and flocculation agent, after amido forms hydrogen bond, by adsorption by integrated for multiple impurity particle macromole floc sedimentation, effect is swept again owing to volume caught by the net of flocculation agent, wadding body magnifies gradually, and in settling process, stick in solution relatively small particle and other wadding body, final formation macrobead floc sedimentation, impel or accelerate their sedimentations, realize under the mechanicals efforts of external world's offer and basis oil separating again. experimental result shows, and the receipts rate of the pretreatment process of waste lubricating oil provided by the invention is higher, and recovered oil quality is better, and have the following advantages: (1) is without the need to adding soda acid, avoiding acid sludge and contaminated wastewater, the waste residue that flocculation process produces is available after carrying out reprocessing makes ink, environmental protection, (2) pre-processing period is short, efficiency height, (3) cost is lower, (4) pre-treatment oil quality is good.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, it should be appreciated that these describe just for the features and advantages of the present invention instead of limiting to the claimed invention are described further.
A kind of pretreated method of waste lubricating oil, comprises the following steps:
1. waste lubricating oil is carried out sedimentation, drying, obtain oil mixture A;
2. described oil mixture A organic solvent carrying out flocculation refining, obtain oil mixture B, described organic solvent refers to hydroxyethylethylene diamine;
3. described oil mixture B is carried out constant temperature sedimentation, separation, obtain pre-treatment oil.
First waste lubricating oil is carried out sedimentation, drying by the present invention, obtains oil mixture A.
In the present invention, described waste lubricating oil is the common waste lubricating oil in this area, and it be there is no particular restriction by the present invention. Waste lubricating oil described in sedimentation of the present invention, mainly utilizes oil to be separated with the density difference of mechanical impurity, removes macrobead mechanical impurity wherein; Described sedimentation is preferably natural subsidence, and the time of described natural subsidence is preferably 19��24h, and simple to operate, impurity-eliminating effect is good; Described drying preferably carries out in thermostatic drying chamber, it is preferable that temperature is 70��80 DEG C, it is preferable that the time is 1��4h.
Described organic solvent refers to hydroxyethylethylene diamine.
Time refining, described oil mixture A, with hydroxyethylethylene diamine, is carried out flocculation refining by the present invention, and waste lubricating oil is had good flocculating effect by described solvent, and the receipts rate of the recovered oil that the present invention obtains can be made higher, and quality is better.
In the present invention, described refining temperature is preferably 50��80 DEG C, it is more preferable to be 55��75 DEG C; The described refining time is preferably 30��90min, it is more preferable to be 30��85min, it is most preferred that be 30��80min. The present invention refines gentleer when, it is not necessary to the processing condition that High Temperature High Pressure etc. are harsh, and avoids acid sludge and contaminated wastewater, environmental protection, with short production cycle, efficiency height.
After refining end, obtain oil mixture B, wherein comprise lubricating oil, solvent and solid impurity etc.
Described oil mixture B is carried out constant temperature sedimentation, separation by the present invention, obtains pre-treatment oil.
The present invention utilizes constant temperature sedimentation, the main solid impurity removed in described oil mixture B. Described constant temperature sedimentation is not particularly limited by the present invention, and the temperature of described constant temperature sedimentation is 50��80 DEG C, it is more preferable to be 55��75 DEG C; The time preferably 2��7h of described constant temperature sedimentation, it is more preferable to be 2��6h.
After obtaining pre-treatment oil, it is carried out quality index detection. The colourity of gained recovered oil is measured according to China national standard GB/T6540-1986 " petroleum products color assay method "; The content of gained regeneration W/O is measured according to China national standard GB/T8929-2006 " the mensuration distillation method of crude oil water content "; The density of gained recovered oil is measured according to China national standard GB/T2540-1981 " petroleum products density measurement method (pycnometric method) "; Gained regeneration oil viscosity is measured according to China national standard GB/T265-1988 " oil kinematic viscosity measuring method "; The pour point of gained recovered oil is measured according to China national standard GB/T3535-2006 " petroleum products pour point assay method "; Gained regeneration oil flash is measured according to China national standard GB/T3536-2008 " mensuration of petroleum products flash-point and burning-point "; The acid number of gained recovered oil is measured according to China national standard GB/T264-1983 " petroleum product acid value measuring method "; The mechanical impurity of gained recovered oil is measured according to China national standard GB/T511-1988 " petroleum products and additive mechanical impurity assay method (weighting method) "; The carbon residue of gained recovered oil is measured according to China national standard GB/T17144-1997 " petroleum products carbon residue assay method (micromethod) "; The content of sulphur in gained recovered oil is measured according to test method SH/T0689-2000 " the total sulfur content assay methods (ultraviolet fluorescence method) of light hydrocarbon and motor spirit and other oil products "; The nitrogen content of gained recovered oil is measured according to China national standard GB/T9170-1988 " lubricating oil and oil fuel in total nitrogen content assay method (the kirschner method of improvement) ", Zn in gained recovered oil is measured according to test method SH/T0228-1992 " in lubricating oil barium, calcium, zinc-content determination method (atomic absorption spectrometry) ", Ga, the content of Fe, Mg.
Test result shows, and the pre-treatment oil quality that the pretreatment process of waste lubricating oil provided by the invention obtains is improved significantly. The receipts rate of the renovation process of waste lubricating oil provided by the invention is more than 83%, very big degree has saved production cost, it is to increase the economic benefit of regeneration waste lubricating oil.
In addition, the pretreatment process of waste lubricating oil provided by the invention is simple to operate, and processing condition are gentle, with low cost, with short production cycle, environmental protection.
In order to understand the present invention further, below in conjunction with embodiment, the pretreatment process of waste lubricating oil provided by the invention is described in detail.
Following examples waste lubricating oil used is provided by Chongqing Auto repair shop, and flocculation solvent used, purchased from Chemical Reagent Co., Ltd., Sinopharm Group.
Embodiment 1:
100g waste lubricating oil is carried out natural subsidence, after 24h, is placed in the dry 4h of 80 DEG C of thermostatic drying chambers, removes portion of water, isolate large granular impurity, obtain oil mixture A; Pour in the beaker of 250mL after the oil mixture A obtained is cooled, add 1.4g hydroxyethylethylene diamine, then be placed on constant temperature magnetic force heating stirrer, open heater switch and stir switch, be warming up to 75 DEG C, after the refining 80min of constant temperature extraction, stop heating and stir, obtain oil mixture B; The oil mixture B obtained being transferred to separating funnel, puts into thermostat container, control temperature is constant 75 DEG C, after sedimentation 6h, closes thermostat container, obtains pre-treatment oil 87.9g, and receipts rate reaches 87.9%.
Being imported in beaker by the pre-treatment oil obtained after sedimentation, according to method mentioned above, it is carried out quality index test, test result is see table 1, and table 1 is the quality index of waste lubricating oil used in the embodiment of the present invention, gained pre-treatment oil.
Embodiment 2:
100g waste lubricating oil is carried out natural subsidence, after 19h, is placed in the dry 2h of 70 DEG C of thermostatic drying chambers, removes portion of water, isolate large granular impurity, obtain oil mixture A; Pour into after the oil mixture A obtained is cooled in the beaker of 250mL, add 1.1g hydroxyethylethylene diamine, then be placed on constant temperature magnetic force heating stirrer, open heater switch and stir switch, be warming up to 55 DEG C, after the refining 30min of constant temperature extraction, stop heating and stir, obtain oil mixture B; The oil mixture B obtained being transferred to separating funnel, puts into thermostat container, control temperature is constant 55 DEG C, after sedimentation 2h, closes thermostat container, obtains pre-treatment oil 83.3g, and receipts rate reaches 83.3%.
Being imported in beaker by the pre-treatment oil obtained after sedimentation, according to method mentioned above, it is carried out quality index test, test result is see table 1, and table 1 is the quality index of waste lubricating oil used in the embodiment of the present invention, gained pre-treatment oil.
The quality index of table 1 oil product
Quality index | The pre-treatment oil of embodiment 1 gained | The pre-treatment oil of embodiment 2 gained | The waste lubricating oil that embodiment is used | Detection method |
Outward appearance | Transparent | Transparent | Opaque | �� |
Colourity | 4 | 4 | 8 | GB/T 6540-1986 |
Moisture/wt% | Trace | Trace | 0.42 | GB/T 8929-2006 |
20 DEG C of density/kg m-3 | 845 | 841 | 886 | GB/T 2540-1981 |
40 DEG C of viscosity/mm2��s-1 | 79.15 | 78.36 | 91.4 | GB/T 265-1988 |
Viscosity index | 98 | 101 | 126 | �� |
Pour point/DEG C | -14 | -13 | -6 | GB/T 3535-2006 |
Flash-point/DEG C | 210 | 212 | 171 | GB/T 3536-2008 |
Acid number/mg KOH g-1 | 0.03 | 0.04 | 1.81 | GB/T 264-1983 |
Mechanical impurity/wt% | 0.03 | 0.03 | 0.35 | GB/T 511-1988 |
Carbon residue/wt% | 0.18 | 0.15 | 1.08 | GB/T17144-1997 |
S/wt% | 0.282 | 0.275 | 0.618 | SH/T 0689-2000 |
N/wt% | 0.037 | 0.041 | 0.072 | GB/T 9170-1988 |
Zn/wt�� | 0.11 | 0.10 | 0.78 | SH/T 0228-1992 |
Ga/wt�� | 0.15 | 0.14 | 0.63 | SH/T 0228-1992 |
Fe/wt�� | 0.48 | 0.42 | 3.27 | SH/T 0228-1992 |
Mg/wt�� | 0.04 | 0.05 | 0.15 | SH/T 0228-1992 |
As shown in Table 1, the pre-treatment quality that the pretreatment process of waste lubricating oil provided by the invention obtains is better.
What finally illustrate is, above embodiment is only in order to illustrate the technical scheme of the present invention and unrestricted, although with reference to better embodiment to invention has been detailed explanation, it will be understood by those within the art that, the technical scheme of the present invention can be modified or equivalent replacement, and not departing from objective and the scope of technical solution of the present invention, it all should be encompassed in the middle of the right of the present invention.
Claims (3)
1. the pretreated method of waste lubricating oil, comprises the following steps:
1. waste lubricating oil is carried out sedimentation, drying, obtain oil mixture A;
2. described oil mixture A organic solvent carrying out flocculation refining, obtain oil mixture B, described organic solvent refers to hydroxyethylethylene diamine;
3. described oil mixture B is carried out constant temperature sedimentation, separation, obtain pre-treatment oil;
The mass ratio of described solvent and described oil mixture A is 1��15:100;
The temperature that described flocculation is refined is 50��80 DEG C;
The time that described flocculation is refined is 30��90min.
2. a kind of pretreated method of waste lubricating oil according to claim 1, it is characterised in that, the temperature of described constant temperature sedimentation is 50��80 DEG C.
3. a kind of pretreated method of waste lubricating oil according to claim 1, it is characterised in that, the time of described constant temperature sedimentation is 2��7h.
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CN104531324A (en) * | 2014-11-28 | 2015-04-22 | 刘林 | Method for producing gear lubricating oil by using recovered lubricating oil |
CN106010766A (en) * | 2016-06-01 | 2016-10-12 | 成都科创诺商贸有限公司 | Regeneration method of waste lubricating oil |
WO2018195543A1 (en) * | 2017-04-21 | 2018-10-25 | Baker Hughes, A Ge Company, Llc | Method of determining the stability reserve and solubility parameters of a process stream containing asphaltenes by joint use of turbidimetric method and refractive index |
CN108219913B (en) * | 2018-02-27 | 2021-07-20 | 浙江绿保再生资源科技有限公司 | Composite flocculant and waste lubricating oil flocculation regeneration process |
CN111876199B (en) * | 2020-08-14 | 2021-03-30 | 肇庆市新荣昌环保股份有限公司 | Method for recycling waste mineral oil |
CN113004941B (en) * | 2021-04-01 | 2022-10-11 | 厦门市汉臻能源科技有限公司 | Industrial purification method of waste engine oil |
CN114724639B (en) * | 2022-06-10 | 2022-09-16 | 国家超级计算天津中心 | Preprocessing acceleration method, device, equipment and storage medium |
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CN1951833A (en) * | 2005-10-21 | 2007-04-25 | 广州市佳境水处理技术工程有限公司 | Organic-inorganic copolymerized decolorized flocculant and its preparation method |
CN101623898A (en) * | 2009-04-28 | 2010-01-13 | 江西赛维Ldk太阳能高科技有限公司 | Chemical recovery method for mortar in wire cutting technology |
CN103266008A (en) * | 2013-05-30 | 2013-08-28 | 山东信诺润滑油有限公司 | Regenerating method for waste lubricating oil |
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CN1951833A (en) * | 2005-10-21 | 2007-04-25 | 广州市佳境水处理技术工程有限公司 | Organic-inorganic copolymerized decolorized flocculant and its preparation method |
CN101623898A (en) * | 2009-04-28 | 2010-01-13 | 江西赛维Ldk太阳能高科技有限公司 | Chemical recovery method for mortar in wire cutting technology |
CN103266008A (en) * | 2013-05-30 | 2013-08-28 | 山东信诺润滑油有限公司 | Regenerating method for waste lubricating oil |
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