CN102453494A - Method of ultrasound-enhanced supercritical extraction of oil sludge - Google Patents
Method of ultrasound-enhanced supercritical extraction of oil sludge Download PDFInfo
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- CN102453494A CN102453494A CN2010105140471A CN201010514047A CN102453494A CN 102453494 A CN102453494 A CN 102453494A CN 2010105140471 A CN2010105140471 A CN 2010105140471A CN 201010514047 A CN201010514047 A CN 201010514047A CN 102453494 A CN102453494 A CN 102453494A
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Abstract
The invention discloses a method of ultrasound-enhanced supercritical extraction of oil sludge. Oil sludge and extractants are added into a supercritical extraction device with an enhanced ultrasound device, and the supercritical extraction pressure and the supercritical extraction temperature are set for supercritical extraction. Compared with the prior art, the technology of the ultrasound-enhanced supercritical extraction is adopted in the method, so the extraction pressure and temperature are reduced, the extraction time is shortened, and finally the extraction efficiency is improved.
Description
Technical field
The present invention relates to treatment process, particularly adopt extracting process to separate the method for greasy filth oily sludge.
Background technology
Greasy filth mainly is meant because the oily sludge of formation such as the crude oil that causes of a variety of causes or other oil product and earth, and the oily sediment that system takes out of in the ordinary production of oil field etc., be a kind of solid waste that is rich in MO, staple is crude oil, Ni Heshui.The solid particulate size can be from not enough micron to several inches, and great majority are between 1 to 100 micron, and crude oil kind, refinery structure and operational condition are depended in oil composition, and the composition of mud possibly change in time and change.Usually contain certain crude oil (concentration quality 5%～80%), heavy metal ion (like iron, copper, nickel etc.) and inorganic salts (concentration quality 5%～20%) compound etc. in the mud.Generally contain materials such as benzene series thing, phenols in these greasy filth; And follow stench and toxicity; If directly contact with physical environment, can make that the soil poisons, acidifying or alkalization, cause the change of soil and soil structure; Hinder plant root growth and can cause bigger pollution, also mean the waste of petroleum resources simultaneously water body and vegetation.
By national Hazardous wastes register, greasy filth is classified as Hazardous wastes, and it just attracts great attention to the chronicity and the potentiality of environmental hazard.Carrying out greasy filth management and Study of Prevention Technology is a vital task of present national environmental protection work.Therefore, how carrying out innoxious and recycling to these oily sludges, also is the important environmental issue that pendulum needs to be resolved hurrily in face of oil refining industry.
The technology of handling oily sludge at present mainly contains resource recovery, harmless treatment and comprehensive utilization technique etc.Resource recycling technology comprises solvent extration, WATER-WASHING METHOD, micro emulsion washing, breakdown of emulsion method etc.Greasy filth harmless treatment treatment technology comprises immobilization processing, technology such as biological treatment, burning.Comprehensive utilization technique comprises that thermolysis, brickmaking are paved the way and other purposes.The treatment technology of greasy filth is varied, and every kind of method all has separately the relative merits and the scope of application.Along with the increasingly stringent of environmental regulation and perfect, oil field oil-containing silt particle treatment technology will attract great attention, the inexorable trend that oily sandy sludge is innoxious, resource utilization, comprehensive utilization treatment technology will become the development of oil sludge and sand treatment technology.
Solvent extration is use always in the greasy filth treatment technology a kind of; Its utilization " similar mixing " principle; Select appropriate organic solvent to make extraction agent; After organism come out by solvent extraction from greasy filth, from mixture, separate solvent through distillation and to recycle, the crude oil of recovery then is used for freshening.
US484271 adopts extraction oxidation oxidation style that oily sludge is handled, and in mud, adds a kind of light hydrocarbon earlier and makes extraction agent, and after extraction, oily and most of organism is removed, and residual mud is used HNO
3Oxide treatment under 200～375 ℃ and condition of normal pressure.
CN02133117.0 adopts the technical finesse oily sludge of " extraction heat-dehydration-solid-liquid separation "; Oily sludge is carried out mechanical dehydration, mix and preheating with extraction solvent oil then, carry out extraction heat-processed after mixing; Carry out solid-liquid separation then; Liquid phase gets into coker, and solid phase can be used as fuel, and the vapour phase of extraction heat-dehydration is carried out oily water separation after condensation.This procedure is simple, need not specific installation, and investment and process cost are low, not only effectively handled oily sludge, and wherein valuable components are fully utilized, and can not give the after-treatment device deleterious impact simultaneously.
The advantage of solvent extration is that the processing oily sludge is more thorough, can most of petroleum substance be extracted and reclaim.But owing to extraction agent costs an arm and a leg, and certain loss is arranged in treating processes, so the extraction cost is higher, this has also restricted the application of solvent extration on greasy filth separates.
Supercritical extraction is a kind of novel extraction stripping technique that develops rapidly in the last thirty years.Supercutical fluid is meant that temperature and pressure is in critical temperature and the above fluid of emergent pressure.Supercutical fluid is the special fluid between gas and liquid; Have the dual rerum natura of gas and liquid concurrently; Its density approaches density of liquid, liquid and solid dissolving power are approached common liquid solvent, and viscosity and velocity of diffusion approaches common gases.Therefore, supercutical fluid has perviousness and stronger dissolving power preferably, and very high rate of mass transfer and reach the ability of extraction equilibrium very soon.Supercritical extraction is exactly this specific character extracting and separating material that utilizes supercutical fluid, makes supercutical fluid become common gases by isothermal step-down or the isobaric method that heats up then, can extraction agent be separated with material to be separated matter.
The supercritical extraction stripping technique is compared with traditional solvent extraction and separation method at aspects such as dissolving power, transmission performance and solvent recuperation all has many advantages: it has the dissolving power close with the common liq solvent. and have the transmission characteristic the same with gas.Promptly, can reach balance quickly than liquid solvent quick permeation; Can select that chemicalstability is good for use, critical temperature as extraction agent, substitutes the traditional poisonous solvent near normal temperature, nontoxic, non-corrosive material, really realizes the production process greenization; Its extractability depends on fluid density, can come to control with comparalive ease through regulating main operating parameters (temperature and pressure); Solvent recuperation is simple and convenient. through isothermal step-down or isobaric the intensification. and extract just can separate with extraction agent, and extraction agent only needs compression again just to can be recycled, and saves the energy.
Avila
M.A [Separation Science and Technology; 2007; 42 (10): 2327-2345]. wait and utilize a kind of special supercritical fluid extraction equipment; Adopt overcritical ethane extraction agent from the petroleum tank bed mud, to extract hydrocarbon; Research thinks that maximum percentage extraction is corresponding to the pressure and temperature of high solvent density, the obvious enrichment of hydrocarbon component of extraction.But because the emulsification degree of greasy filth is high, solid impurity is many, and solid water-oil-rock steady structure for complicacy adopts the extraction or the supercritical extraction method of routine, need the extraction time long, extraction efficiency is low, has limited its application.
Summary of the invention
To the deficiency of prior art, the invention provides the method that a kind of supercritical extraction separates greasy filth, the inventive method has the high advantage of extraction efficiency.
The method of ultrasound-enhanced supercritical extraction greasy filth of the present invention comprises: greasy filth and extraction agent get into and have the supercritical extraction unit of strengthening Vltrasonic device, set supercritical extraction pressure and supercritical extraction temperature, carry out supercritical extraction.Extraction agent is selected carbonic acid gas, methane, ethane, propane or ethene, is preferably carbonic acid gas or ethane.
Extraction agent and greasy filth amount ratio are that every gram greasy filth uses 20～50ml extraction agent, and supercritical extraction pressure is 3～8MPa, and the supercritical extraction temperature is 30～100 ℃, and the supercritical extraction time is 2～6h.
According to the described method of claim 1; It is characterized in that: ultrasonic frequency is 20～40kHz; Ultrasonic power density is 40～100W/L (being the ultrasonic power that every liter of material uses), ultrasonic continuous irradiation or intermitant irradiation, and the quiescent interval during intermitant irradiation is (6～12s)/(6～12s)
Material after the extraction gets into primary separator, second-stage separator separates, and recycles after the solvent gasification, and extract is emitted from the separator bottom, gets into water-and-oil separator and separates, and water carries out WWT.After oil phase is settlement separate, obtain oil content and solids, solids acts as a fuel through the de-oiling drying or after solidifying.But gained oil content freshening factory makes processing treatment.
Supercritical extraction can adopt operate continuously, also can adopt batch operation.
When the present invention is directed to greasy filth extraction or supercritical extraction, because the extraction that the greasy filth Stability Analysis of Structures causes difficulty, the extraction time is long, and the deficiency that extraction efficiency is low on the basis of suitable supercritical extraction, increases intensified by ultrasonic wave.The ultrasound-enhanced supercritical abstraction technique is an additional ultrasonic field in supercritical extraction, thereby reduces extracting pressure and temperature, shortens the extraction time, finally improves percentage extraction.For greasy filth, owing to be stable oil-water-fixing structure, adopt suitable ultrasonic field, can make this rock steady structure produce vibration, disintegrate, accelerated interphase mass transfer speed, help the carrying out that extract, and then improved extraction efficiency.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
The supercritical fluid extraction influence factor mainly contains extraction conditions, comprises pressure, temperature, time etc.; The kind of raw material properties and supercutical fluid.Wherein the selection of supercutical fluid is most important.In the supercritical fluid extraction process, require supercutical fluid to have good solubility ability and good selectivity.From the consideration of safety, economy and environmental protection, also has following requirement simultaneously for supercutical fluid; Chemical property is stable, and nontoxicity and non-corrosiveness are nonflammable and non-explosive; The service temperature of supercutical fluid should approach normal temperature, so that save energy, and service temperature is lower than treat the decomposition temperature of separated component; The working pressure of supercutical fluid should be low as much as possible, to reduce the power consumption of compressor; Wide material sources, low price.In conjunction with the character of greasy filth, the present invention selects carbonic acid gas, methane, ethane, propane and other low molecule alkane, ethene and other low-molecular olefine etc. as the supercritical extraction agent, and its critical data is as shown in table 1.
The critical data of table 1 part supercritical fluid solvent
The variation of supercritical flow volume density directly influences effect of extracting in the extraction process, and extracting pressure is the important parameter that influences supercritical phase density.According to the variation of extracting pressure, can supercutical fluid be divided three classes.When being high pressure; The dissolving power of supercutical fluid is strong, can dissolve all the components to greatest extent, and the low pressure critical zone only can be extracted diffluent composition or removed objectionable constituent; The slective extraction of middle nip is asked high-low pressure, can select suitable pressure effectively to extract according to the requirement of materials abstraction.The present invention is directed to the character of greasy filth, and the extraction agent character of selecting, consider additional ultrasound-enhanced effect simultaneously, the extracting pressure of selection is 3～8MPa.
Near stagnation point low pressure area, though elevated temperature can improve the volatility and the diffusibility of separated portion, the density that is not enough to replenish supercutical fluid raises with temperature and the institute that sharply descends causes dissolving power to descend.In the high pressure area, the density of supercutical fluid is big, and compressibility is little, and this moment, elevated temperature can improve vp and the spread coefficient of treating separated portion, thereby had improved the dissolving power of solute.Adopt ultrasound-enhancedly to the character of greasy filth and the present invention, adopt 30～70 ℃ of lower extraction temperature.
Specific embodiment 1:
With greasy filth at the bottom of certain refinery's oil tank is the example explanation specific embodiment of the invention.Greasy filth oil-containing 65wt%, moisture 18wt%, all the other are solid matter.Select CO
2As the supercritical extraction agent.Ultrasonic power density is 100W/L, and frequency is 20kHz, and radiation mode is 6s/6s (ultrasonic continuous irradiation time/ultrasonic quiescent interval).The consumption of extraction agent and greasy filth is 30ml/g (a greasy filth raw material).
Greasy filth is sent into supercritical extraction reactor after the mechanical stirring dehydration.Ultransonic schedule of reinforcement adopts built-in insert, and ultrasonic transducer directly places extractor, and ultrasonic generator will transfer superaudible electric energy to and pass to transverter, be converted into ultrasonic frequency mechanical energy to electric energy by transverter again.From storage tank (CO
2) the liquid CO that comes out
2Purify through filtering system, be transported to preheating in the preheater through HPP then, be preheated to design temperature after, get into to reach in the extraction kettle and set extracting pressure and extraction temperature, extraction temperature is 30～50 ℃, extracting pressure is 3～6MPa, the extraction time is 2h.CO in extraction kettle
2Contact with raw material, be extracted composition and be dissolved in CO
2In extract.Extract remainder carry out settlement separate after, obtain a little oil content and solids, act as a fuel after solids solidifies.Extract is with CO
2Fluid successively gets into primary separator and second-stage separator, extract and CO
2Separate, receive through receiving system; CO
2Then isolate and reuse from second-stage separator.Percentage extraction through strengthening ultrasonic supercritical extraction greasy filth is 95%-99% (quality) under different operating conditions.Extract is emitted from the separator bottom, gets into water-and-oil separator and separates, and water carries out WWT.But oil phase freshening factory gets into catalytic cracking or coking process.
Specific embodiment 2:
With greasy filth at the bottom of certain refinery's oil tank is the example explanation specific embodiment of the invention.Greasy filth oil-containing 65%, moisture 18%, all the other are solid matter.Select ethane as the supercritical extraction agent.Extraction temperature is 30～100 ℃, and extracting pressure is 5～8MPa, and the consumption of extraction agent and greasy filth is 40ml/g (a greasy filth raw material), and the extraction time is 2.5h.Ultrasonic power density is 80W/L, and frequency is 20kHz, and radiation mode is 6s/6s (ultrasonic continuous irradiation time/ultrasonic quiescent interval).Technical process is with embodiment 1, and the percentage extraction of greasy filth is 95%-99% (quality).
Claims (6)
1. the method for ultrasound-enhanced supercritical extraction greasy filth, it is characterized in that: greasy filth gets into extraction agent and has the supercritical extraction unit of strengthening Vltrasonic device, and setting supercritical extraction pressure and supercritical extraction temperature are carried out supercritical extraction.
2. according to the described method of claim 1, it is characterized in that: extraction agent is selected carbonic acid gas, methane, ethane, propane or ethene.
3. according to claim 1 or 2 described methods; It is characterized in that: extraction agent and greasy filth amount ratio are that every gram greasy filth uses 20～50ml extraction agent; Supercritical extraction pressure is 3～8MPa, and the supercritical extraction temperature is 30～100 ℃, and the supercritical extraction time is 2～6h.
4. according to the described method of claim 1, it is characterized in that: ultrasonic frequency is 20～40kHz, and ultrasonic power density is 40～100W/L, ultrasonic continuous irradiation or intermitant irradiation, and the quiescent interval during intermitant irradiation is (6～12s)/(6～12s).
5. according to the described method of claim 1; It is characterized in that: the material after the extraction gets into primary separator, second-stage separator separates, and recycles after the solvent gasification, and extract is emitted from the separator bottom; The entering water-and-oil separator separates, and water carries out WWT.
6. according to the described method of claim 1, it is characterized in that: supercritical extraction adopts operate continuously, perhaps adopts batch operation.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103145306A (en) * | 2013-03-20 | 2013-06-12 | 北京昊诚油气科技有限公司 | Combined process and device for processing oily sludge through supercritical extraction method |
| CN103395953A (en) * | 2013-08-12 | 2013-11-20 | 江苏君鑫谊石油机械有限公司 | Oil-sludge separation method based on CO2 supercritical extraction method |
| CN103450920A (en) * | 2013-09-13 | 2013-12-18 | 中国农业大学 | Method for increasing heavy oil yield by treating biological crude oil with ultrasonic wave |
| CN103979756A (en) * | 2014-05-27 | 2014-08-13 | 陕西延长石油（集团）有限责任公司 | Method for tempering oily sludge by using supercritical fluid through rapid swelling |
| CN104764813A (en) * | 2014-12-15 | 2015-07-08 | 青岛科技大学 | Kinetic rapid determination method for removing residual solvent in thermosensitive solid drug in virtue of high pressure CO2 |
| CN105174575A (en) * | 2015-10-19 | 2015-12-23 | 无锡清杨机械制造有限公司 | Method for purifying sewage by utilizing ultrasonic extraction technique |
| CN105330124A (en) * | 2015-11-25 | 2016-02-17 | 东南大学 | Microwave radiation solvent extraction combination deep dehydration method and device applied to biological solid matter |
| CN106479556A (en) * | 2015-08-31 | 2017-03-08 | 通用电气公司 | The system and method for recovering hydrocarbon |
| CN108644787A (en) * | 2018-04-11 | 2018-10-12 | 中国石油大学(华东) | Oily sludge extraction-separation-drying-burning integral process system |
| CN109173333A (en) * | 2018-09-30 | 2019-01-11 | 湖北中油科昊机械制造有限公司 | A kind of novel carbon dioxide extraction element |
| CN110451745A (en) * | 2019-07-10 | 2019-11-15 | 合肥通用机械研究院有限公司 | A kind of oil base drilling wastes supercritical processing system |
| CN110624273A (en) * | 2019-10-25 | 2019-12-31 | 北京和荣工程技术有限公司 | Supercritical CO improving agent2Method and system for extracting oil sludge extraction rate |
| CN112876036A (en) * | 2021-02-23 | 2021-06-01 | 扬州阿鲁达环境科技有限公司 | Ultrasonic-based oily sludge treatment system and process |
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| CN103145306A (en) * | 2013-03-20 | 2013-06-12 | 北京昊诚油气科技有限公司 | Combined process and device for processing oily sludge through supercritical extraction method |
| CN103145306B (en) * | 2013-03-20 | 2018-07-17 | 北京昊诚油气科技有限公司 | A kind of group technology and device of supercritical extraction processing oily sludge |
| CN103395953A (en) * | 2013-08-12 | 2013-11-20 | 江苏君鑫谊石油机械有限公司 | Oil-sludge separation method based on CO2 supercritical extraction method |
| CN103450920A (en) * | 2013-09-13 | 2013-12-18 | 中国农业大学 | Method for increasing heavy oil yield by treating biological crude oil with ultrasonic wave |
| CN103979756A (en) * | 2014-05-27 | 2014-08-13 | 陕西延长石油（集团）有限责任公司 | Method for tempering oily sludge by using supercritical fluid through rapid swelling |
| CN103979756B (en) * | 2014-05-27 | 2015-05-20 | 陕西延长石油（集团）有限责任公司 | Method for tempering oily sludge by using supercritical fluid through rapid swelling |
| CN104764813A (en) * | 2014-12-15 | 2015-07-08 | 青岛科技大学 | Kinetic rapid determination method for removing residual solvent in thermosensitive solid drug in virtue of high pressure CO2 |
| CN106479556A (en) * | 2015-08-31 | 2017-03-08 | 通用电气公司 | The system and method for recovering hydrocarbon |
| CN106479556B (en) * | 2015-08-31 | 2021-02-26 | 通用电气公司 | System and method for recovering hydrocarbons |
| CN105174575A (en) * | 2015-10-19 | 2015-12-23 | 无锡清杨机械制造有限公司 | Method for purifying sewage by utilizing ultrasonic extraction technique |
| CN105330124A (en) * | 2015-11-25 | 2016-02-17 | 东南大学 | Microwave radiation solvent extraction combination deep dehydration method and device applied to biological solid matter |
| CN105330124B (en) * | 2015-11-25 | 2018-04-24 | 东南大学 | A kind of method and device of microwave radiation solvent extraction combination deep dehydration for biosolids material |
| CN108644787A (en) * | 2018-04-11 | 2018-10-12 | 中国石油大学(华东) | Oily sludge extraction-separation-drying-burning integral process system |
| CN109173333A (en) * | 2018-09-30 | 2019-01-11 | 湖北中油科昊机械制造有限公司 | A kind of novel carbon dioxide extraction element |
| CN110451745A (en) * | 2019-07-10 | 2019-11-15 | 合肥通用机械研究院有限公司 | A kind of oil base drilling wastes supercritical processing system |
| CN110451745B (en) * | 2019-07-10 | 2021-11-23 | 合肥通用机械研究院有限公司 | Oil-based drilling waste supercritical treatment system |
| CN110624273A (en) * | 2019-10-25 | 2019-12-31 | 北京和荣工程技术有限公司 | Supercritical CO improving agent2Method and system for extracting oil sludge extraction rate |
| CN112876036A (en) * | 2021-02-23 | 2021-06-01 | 扬州阿鲁达环境科技有限公司 | Ultrasonic-based oily sludge treatment system and process |
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