CN104046375B - Microwave-assisted supercritical CO 2the system and method for extraction crude oil from oil sand - Google Patents
Microwave-assisted supercritical CO 2the system and method for extraction crude oil from oil sand Download PDFInfo
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- CN104046375B CN104046375B CN201410258254.3A CN201410258254A CN104046375B CN 104046375 B CN104046375 B CN 104046375B CN 201410258254 A CN201410258254 A CN 201410258254A CN 104046375 B CN104046375 B CN 104046375B
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Abstract
The invention discloses a kind of microwave-assisted supercritical CO
2the system and method for extraction crude oil from oil sand, system comprises extraction kettle, microwave generator, separator, gas purifier, surge tank, entrainment agent storage tank etc.Treatment process is: oil-sand delivers to extraction kettle by e Foerderanlage, simultaneously CO
2, entrainment agent enters surge tank, in surge tank, mixture enters extraction kettle, closes extraction kettle entrance end valve; Open microwave generator, after reaching extraction temperature in still, stay for some time, open still bottom valve, discharge sand, open still top outlet valve, gaseous fluid enters separator through throttling valve; Crude oil is discharged in separator bottom outlet, and top gas, through cleaner, is back to surge tank.Operation system setting at least two extraction kettles, can realize running continuously by alternate operation.
Description
Technical field
The present invention relates to a kind of oil-sand separation technology, be specifically related to a kind of supercritical CO
2the system and method for extraction crude oil from oil sand.
Background technology
Along with the continuous increase of global demand of petroleum, conventional oil resource can not meet the quick growth of petroleum demand, and people start sight to turn to non-conventional oil resource.Oil-sand, as the main source of non-conventional oil resource, plays a part very important in world's energy resource supply.According to the research of US Geological Survey, tar sand oil mining resources amount is about 103.51 × 10 in the world
9m
3, account for that world petroleum resource can adopt total amount 32%.At present, to the research and development of oil-sand, all over the world all in acceleration, along with the raising of exploratory development technology, its proportion accounting for the global hydro carbons energy will constantly increase.
Oil-sand ore deposit is generally imbedded in earth's surface to the dark underground of 760m, generally adopts opencast mode to exploit both at home and abroad at present.But the oil-sand had an opencast mining of out need set up corresponding oil/sand separator.Existing oil-sand separation technology has hot alkali wash and solvent extration.But these two kinds of methods all have the defect of a bit, as hot alkali wash need soak with a large amount of high temperature alkaline solutions, reached the object of greasy filth separation by the method for washing.This method cost of winning is higher, and labour intensity is comparatively large, and water resource waste comparatively greatly, and produces a large amount of sewage, causes secondary pollution.Solvent extration complex process, facility investment is excessive, and due to solvent oil flash-point very low and very easily burn, there is larger security against fire hidden danger during use.
Patent documentation CN103395953A discloses a kind of CO
2supercritical extraction oil sludge separation method, comprises extraction solvent, solid-liquid separation, earth discharge, pneumatic separation and crude oil collection process.CO is mentioned in this invention
2there is not chemical reaction in extraction process, and tasteless, nontoxic, and security is very good, simultaneously CO
2gas price is cheap, and purity is high, easily extracts, and reusable.
Supercritical CO
2extraction process utilizes supercritical CO
2dissolving power and the relation of its density, namely utilize pressure and temperature to supercritical CO
2the impact of dissolving power is carried out.In the supercritical state, by supercritical CO
2contact with material to be separated, make it selectively the composition of polarity size, boiling point height and molecular size range be extracted successively.Then the method by decompression or cooling makes supercutical fluid become common gases, is extracted material and then separates out completely or substantially, thus reach the object of separating-purifying.
But supercritical CO
2there is Selective dissolution, excellent solvability is shown to lower molecular weight, low polarity, lipotropy, lower boiling composition such as volatile oil, hydrocarbon, ester, ether, epoxy compounds etc.; But to having the compound of polar group (-OH ,-COOH etc.), polar group is more, just more difficult extraction, therefore polyvalent alcohol, polyprotonic acid and polyhydric aromatoising substance are all insoluble in supercritical CO
2; In addition, the compound high to molecular weight, the more high more difficult extraction of molecular weight, the macromolecular compound of molecular weight more than 500 is almost insoluble.And crude oil from oil sand is except containing except a large amount of lipotropy alkane, also containing a certain amount of heavy oil and colloid, the content of these materials in crude oil is generally at 5wt% ~ 20wt%, and its molecular weight is comparatively large (300 ~ 1000) then, at supercritical CO
2in solubleness lower.Therefore, supercritical CO is adopted
2during technology extraction crude oil from oil sand, if do not take other measures to improve its extraction efficiency to macromolecular substance, supercritical CO
2the technical superiority of extraction then can not well be played; In addition, do not extract oil-sand discharge thoroughly and also can cause secondary pollution.
Summary of the invention
The object of this invention is to provide a kind of supercritical CO of efficient, economy, non-secondary pollution
2extraction oil sand separation technology.For supercritical CO
2to the low-solubility of polar organic matter and high-molecular-weight organic material, take to supercritical CO
2in add three components, i.e. entrainment agent, improve the solubleness of polymer substance; Adopt the method for microwave auxiliary extraction simultaneously, utilize the characteristics such as the fluctuation of microwave, high frequency, penetrance, physics breakdown of emulsion and heating are carried out to oil-sand simultaneously, improve supercritical CO
2extraction efficiency.
For achieving the above object, the present invention takes following technical scheme to be achieved:
A kind of microwave-assisted supercritical CO
2the system of extraction crude oil from oil sand, it is characterized in that, comprise at least two extraction kettles, microwave generator is all equipped with in each extraction kettle periphery, the top inlet of each extraction kettle sends into oil-sand by e Foerderanlage, each extraction kettle bottom inlet is communicated with surge tank outlet at bottom by high-pressure compressor, and sand removing hole is established in each extraction kettle lower end; An import of described surge tank is by low pressure air compressor and CO
2storage tank is communicated with, and another import is communicated with entrainment agent storage tank by liquid compression pump; Each extraction kettle is communicated with separator top inlet by throttling valve, and CRUDE OIL EMISSIONS mouth is established in separator bottom, and separator top exit is communicated with gas purifier, and gas purifier top exit is communicated with the 3rd import of surge tank.
In such scheme, an import and a preheater that the connecting tube of low-pressure gas transferpump is connected of described surge tank.
A kind of microwave-assisted supercritical CO
2the method of extraction crude oil from oil sand, adopts aforementioned system to realize, it is characterized in that, comprise the steps:
(1) by CO
2from CO
2storage tank sends into surge tank through low-pressure gas compression pump; Entrainment agent is pumped to surge tank from entrainment agent storage tank through liquid compression, oil-sand is delivered to an extraction kettle, close other extraction kettle terminal valve, system starts;
(2) CO in surge tank
2and entrainment agent mixture sends into the extraction kettle that oil-sand is housed through high-pressure compressor; Open the microwave generator of this extraction kettle periphery, after reaching extraction temperature in still, stay for some time, open upper outlet valve, gaseous fluid is entered separator through throttling valve, open still bottom valve, discharge the sand after extraction;
(3) crude oil is discharged in separator bottom outlet, and top is containing CO
2and the gas of entrainment agent is back to surge tank through gas purifier, completes an extraction kettle and the intermittence of oil-sand is extracted;
(4) after this, second extraction kettle ..., until last extraction kettle respectively repeats steps the operation of (1) ~ (3) successively;
(5) again from first extraction kettle, the operation of repeating step (1) ~ (3), makes oil-sand cycling extraction successively in multiple stage reactor, makes system enter the continuous operation phase.
In aforesaid method, the irradiation frequency of described microwave generator is 300 ~ 8000MHz.Described extraction kettle interior reaction temperature controls at 35 ~ 75 DEG C, and pressure-controlling is at 7 ~ 30MPa.
Temperature in described separator controls at 35 ~ 75 DEG C, and pressure-controlling is at 3 ~ 15MPa.
Described entrainment agent is methyl alcohol, ethanol, acetone or ethyl acetate.
Advantage of the present invention is, utilizes microwave to heat material, in heat-processed, achieve efficient breakdown of emulsion simultaneously, is conducive to improving CO
2extraction efficiency; Simultaneously at supercritical CO
2in add entrainment agent, can supercritical CO be improved
2to the solubleness of high-molecular-weight organic material, improve extraction efficiency further.In operation, adopt multiple stage reactor periodic running successively, ensure that the continuity of whole system is run, achieve the separation of efficient, clean, less energy-consumption of oil, sand.The present invention opens up new oil supply line by being conducive to, and alleviates the oil gas relation between supply and demand be becoming tight current day.
Accompanying drawing explanation
Fig. 1 is the structural representation of present system.
In Fig. 1: 1, rotary conveyor; 2, the first extraction kettle; 3, the first microwave generator; 4, the second extraction kettle; 5, the second microwave generator; 6, valve; 7, CO
2storage tank; 8, low pressure air compressor; 9, preheater; 10, surge tank; 11, entrainment agent storage tank; 12, liquid compression pump; 13, high-pressure compressor; 14, throttling valve; 15, separator; 16, gas purifier.
Embodiment
Below in conjunction with accompanying drawing and a specific embodiment, the present invention is described in further detail:
With reference to Fig. 1, a kind of microwave-assisted supercritical CO
2the system of extraction crude oil from oil sand, comprises two extraction kettles 2,4, two microwave generators 3,5, a preheater 9, separator 15, gas purifier 16, surge tank 10, entrainment agent storage tank 11 etc.
The top inlet of extraction kettle 2,4 connects the rotary conveyor 1 of conveying oil-sand OS by valve 6, extraction kettle 2,4 bottom inlet is communicated with the outlet at bottom of surge tank 10 by high-pressure compressor 13, and the outlet of extraction kettle 2,4 lower end is sand discharge mouth Sand; An import of surge tank is by preheater 9, low pressure air compressor 8 and CO
2storage tank 7 connects, and another import of surge tank is communicated with entrainment agent storage tank 11 by liquid compression pump 12; Extraction kettle 2,4 upper outlet is communicated with separator 15 top inlet by throttling valve 14, and separator lower part outlet is CRUDE OIL EMISSIONS mouth Oil after extraction, and separator top exit is communicated with gas purifier 16, and gas purifier top exit is communicated with the import in the middle part of surge tank.
Adopt a kind of microwave-assisted supercritical CO of Fig. 1 system
2the method of extraction crude oil from oil sand: treatment capacity is 20t/d, and oleaginousness is the oil-sand of 20wt%, system is when starting shooting, and close the second extraction kettle 4 entrance end valve, oil-sand is delivered to the first extraction kettle 2 by rotary conveyor 1, closes extraction kettle top valve; Meanwhile, the CO of 20kg/h
2from CO
2storage tank 7 is compressed to 7.5MPa through low-pressure gas compression pump 8, and is preheated to 50 DEG C through preheater 9, enters surge tank 10; The methyl alcohol (entrainment agent) of 1kg/h is compressed to 7.5MPa from entrainment agent storage tank 11 through liquid compression pump 12, enters surge tank 10, the CO in surge tank 10
2and entrainment agent mixture is compressed to 20MPa through high-pressure compressor 14 and enters the first extraction kettle 2, close the first extraction kettle entrance end valve; Open agitator and the first microwave generator 3 in the first extractive reaction still, microwave exposure frequency is 1000MHz, and temperature in the kettle stops 10min after reaching 65 DEG C; Open the first extraction kettle bottom valve, discharge the sand after extraction; Open the first extraction kettle upper outlet valve, gaseous fluid is depressurized to 7MPa through throttling valve 15 and enters separator 16.After extraction process terminates in the first extraction kettle 2, open the second extraction kettle 4 entrance end valve, oil-sand through rotary conveyor, CO
2and methyl alcohol enters the second extraction kettle 4 through surge tank 10, close the first extraction kettle 2 terminal valve, open the second extraction kettle agitator and the second microwave generator, 10min is stopped equally after temperature in the kettle rises to 65 DEG C, open the second extraction kettle top valve, Top fluidic enters separator through throttling valve 14, and bottom valve opens sediment outflow; Then the first extraction kettle repeats above-mentioned steps, and enter work, two reactor intermittences operate.In separator 15, temperature is 65 DEG C, and pressure is 7MPa, and gas-liquid realizes being separated at this, and crude oil is discharged from outlet at bottom, methyl alcohol and CO
2enter gas purifier 16 from top exit, cleaner 16, built with discolour silica gel and molecular sieve, adsorbs methyl alcohol and CO
2the moisture carried in fluid and other impurity, the methyl alcohol after purification and CO
2return surge tank 10, complete a circulation.After system enters normal operation, preheater quits work, CO
2with methyl alcohol by pump supplement respectively the flow of 0.2kg/h, 0.1kg/h enter surge tank (in this example, a working cycle CO
2be 1% with the rate of consumption of methyl alcohol).
The percentage extraction of this example crude oil can reach 98%, and after process, oil-sand oleaginousness is lower than 1wt%, daily output crude oil 3.9t.
The present invention is not limited to above embodiment, and processing parameter involved in the present invention can adjust as the case may be, as preheater can adopt electrically heated, also can be gas heating, also can be coal-fired heating.CO
2temperature after preheating higher than its critical point temperature (>32 DEG C), after system is normally run, CO
2without the need to preheating, preheater can be stopped transport.At system start-up phase, CO
2the amount entering surge tank is crude content to be extracted and it is at supercritical CO
21 ~ 5 times of middle solubleness ratio, after system is normally run, the CO supplemented
2amount be extraction, the amount that consumes of separation, scavenging process.
The pressure of extraction kettle is in 7 ~ 30MPa adjustment, and temperature is 35 ~ 75 DEG C of adjustment.The irradiation frequency of microwave generator is 300 ~ 8000MHz, and continuously adjustabe.The temperature of separator controls at 35 ~ 75 DEG C, and pressure adjusts within the scope of 3 ~ 15MPa.
Entrainment agent, except with except methyl alcohol, also can adopt the organic solvents such as ethanol, acetone, ethyl acetate.
Claims (7)
1. a microwave-assisted supercritical CO
2the system of extraction crude oil from oil sand, it is characterized in that, comprise at least two extraction kettles, microwave generator is all equipped with in each extraction kettle periphery, the top inlet of each extraction kettle sends into oil-sand by e Foerderanlage, each extraction kettle bottom inlet is communicated with surge tank outlet at bottom by high-pressure compressor, and sand removing hole is established in each extraction kettle lower end; An import of described surge tank is by low pressure air compressor and CO
2storage tank is communicated with, and another import is communicated with entrainment agent storage tank by liquid compression pump; Each extraction kettle is communicated with separator top inlet by throttling valve, and CRUDE OIL EMISSIONS mouth is established in separator bottom, and separator top exit is communicated with gas purifier, and gas purifier top exit is communicated with the 3rd import of surge tank.
2. microwave-assisted supercritical CO as claimed in claim 1
2the system of extraction crude oil from oil sand, is characterized in that, an import and a preheater that the connecting tube of low-pressure gas transferpump is connected of described surge tank.
3. a microwave-assisted supercritical CO
2the method of extraction crude oil from oil sand, adopts microwave-assisted supercritical CO described in claim 1
2the system of extraction crude oil from oil sand realizes, and it is characterized in that, comprises the steps:
(1) by CO
2from CO
2storage tank sends into surge tank through low-pressure gas compression pump; Entrainment agent is pumped to surge tank from entrainment agent storage tank through liquid compression, oil-sand is delivered to an extraction kettle, close other extraction kettle terminal valve, system starts;
(2) CO in surge tank
2and entrainment agent mixture sends into the extraction kettle that oil-sand is housed through high-pressure compressor; Open the microwave generator of this extraction kettle periphery, after reaching extraction temperature in still, stay for some time, open upper outlet valve, gaseous fluid is entered separator through throttling valve, open still bottom valve, discharge the sand after extraction;
(3) crude oil is discharged in separator bottom outlet, and top is containing CO
2and the gas of entrainment agent is back to surge tank through gas purifier, completes an extraction kettle and the intermittence of oil-sand is extracted;
(4) after this, second extraction kettle ..., until last extraction kettle respectively repeats steps the operation of (1) ~ (3) successively;
(5) again from first extraction kettle, the operation of repeating step (1) ~ (3), makes oil-sand cycling extraction successively in multiple stage reactor, makes system enter the continuous operation phase.
4. microwave-assisted supercritical CO as claimed in claim 3
2the method of extraction crude oil from oil sand, it is characterized in that, the irradiation frequency of described microwave generator is 300 ~ 8000MHz.
5. microwave-assisted supercritical CO as claimed in claim 3
2the method of extraction crude oil from oil sand, it is characterized in that, described extraction kettle interior reaction temperature controls at 35 ~ 75 DEG C, and pressure-controlling is at 7 ~ 30MPa.
6. microwave-assisted supercritical CO as claimed in claim 3
2the method of extraction crude oil from oil sand, it is characterized in that, the temperature in described separator controls at 35 ~ 75 DEG C, and pressure-controlling is at 3 ~ 15MPa.
7. microwave-assisted supercritical CO as claimed in claim 3
2the method of extraction crude oil from oil sand, it is characterized in that, described entrainment agent is methyl alcohol, ethanol, acetone or ethyl acetate.
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| CN104724894A (en) * | 2015-03-24 | 2015-06-24 | 南通睿智超临界科技发展有限公司 | Method for processing oily sludge through supercutical fluid |
| CN104946383B (en) * | 2015-04-30 | 2018-07-03 | 江苏江大源生态生物科技有限公司 | A kind of supercritical CO2The method that composite microwave auxiliary extraction prepares ganoderma lucidum spore oil |
| CN105126382A (en) * | 2015-08-11 | 2015-12-09 | 上海震樨机电科技发展有限公司 | Supercritical extraction three extraction kettle combination process |
| CN107513397A (en) * | 2016-06-17 | 2017-12-26 | 中国石油化工股份有限公司 | The method and its application of n-alkane in a kind of extraction geological sample |
| CN109651041B (en) * | 2017-10-11 | 2022-08-19 | 中国石油化工股份有限公司 | Preparation method of low-carbon olefin |
| CN109652112B (en) * | 2017-10-11 | 2023-11-10 | 中国石油化工股份有限公司 | Method for reducing viscosity of high-viscosity oil |
| 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 |
| CN110484346B (en) * | 2019-09-18 | 2022-03-15 | 中国人民解放军陆军勤务学院 | Based on supercritical CO2Method for regenerating used lubricating oil |
| 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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