CN107219322A - Dynamic determines CO2The method of crude oil effect generation amount of asphaltene precipitation - Google Patents

Dynamic determines CO2The method of crude oil effect generation amount of asphaltene precipitation Download PDF

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Publication number
CN107219322A
CN107219322A CN201710376823.8A CN201710376823A CN107219322A CN 107219322 A CN107219322 A CN 107219322A CN 201710376823 A CN201710376823 A CN 201710376823A CN 107219322 A CN107219322 A CN 107219322A
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China
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crude oil
reactor
asphaltene
precipitation
asphaltene precipitation
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CN201710376823.8A
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Inventor
赵东锋
殷丹丹
竺柏康
高建丰
宋付权
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Zhejiang Ocean University ZJOU
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Zhejiang Ocean University ZJOU
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Priority to CN201710376823.8A priority Critical patent/CN107219322A/en
Publication of CN107219322A publication Critical patent/CN107219322A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/02Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using precipitation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00Measuring arrangements characterised by the use of optical techniques
    • G01B11/28Measuring arrangements characterised by the use of optical techniques for measuring areas
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/02Investigating particle size or size distribution
    • G01N15/0205Investigating particle size or size distribution by optical means, e.g. by light scattering, diffraction, holography or imaging
    • G01N15/0227Investigating particle size or size distribution by optical means, e.g. by light scattering, diffraction, holography or imaging using imaging, e.g. a projected image of suspension; using holography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/04Investigating sedimentation of particle suspensions
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N2015/0092Monitoring flocculation or agglomeration

Abstract

CO is determined the invention provides a kind of dynamic2The method of crude oil effect generation amount of asphaltene precipitation, pours into reactor by crude oil by crude oil piston container using the first ISCO pumps, recycles the 2nd ISCO pumps to pass through CO2Piston container is by CO2Reactor is passed through, and CO is controlled using the 2nd ISCO pumps2Pressure, pass through CCD camera and computer Real Time Observation crude oil CO2The image of layer, and the area of asphaltene precipitation and the Size Distribution of particle are determined with image analysis software, the precipitation capacity under a small amount of reservoir conditions is determined by asphaltene deposits amount Indirect Determination, the asphaltene deposits image obtained in previous experiments is demarcated by these measured values, sets up and coating ratio and amount of asphaltene precipitation linear relationship is precipitated in image.Have the beneficial effect that:Apparatus of the present invention are simple, with low cost, easy to operate, can pass through CCD camera and computer Real Time Observation crude oil CO2The image of layer.

Description

Dynamic determines CO2The method of-crude oil effect generation amount of asphaltene precipitation
Technical field
It is specifically that a kind of dynamic determines CO the present invention relates to oil recovering technical field2- crude oil effect generation asphalitine is sunk The method of shallow lake amount.
Background technology
CO2Drive is a kind of very effective method for improving oil recovery factor, and it can not only effectively improve oil recovery factor, Greenhouse gas emissions can also be significantly reduced.In CO2Inject after reservoir, CO2The asphalitine in crude oil can be caused to occur flocculation and heavy Form sediment, the asphalitine of precipitation can also block pore throat, reduce porosity and permeability, change the wetability of rock, to CO2Drive is carried High recovery rate is impacted.Determine CO2CO during drive2It is that research is crucial with amount of asphaltene precipitation caused by crude oil effect.
During carbon dioxide displacement, CO2Dissolving in crude oil occurs the composition of reservoir fluid and the thermodynamic condition of system Many changes, have broken the shakiness that the solid phase components such as colloid, asphalitine in the original dynamic balance state of crude oil, crude oil become It is fixed, it is easily created asphaltene precipitation.
There are a variety of theories in existence form of the asphalitine in crude oil, at present, and asphaltene colloid beam model is generally to accept One of theory.Theory thinks colloid Molecular Adsorption that asphaltene molecules are bound to each other to form in glue core, oil phase on glue core surface The monomer molecule formed in solvated layer, oil phase is in a homeostasis process with colloid molecule.
Asphalitine be in crude oil in the form of dispersion colloid exist, using asphaltene molecules group as core, periphery round Colloid formation micella, micella is dispersed in crude oil system.Pitch mass-energy disperses to exist in crude oil system, it is important to colloid conduct The presence of peptizing agent.When gum level in system is not enough, the thickness low LCL of the solvated layer of micella is thick, cannot form glue Beam, asphaltene molecules will be further combined with bigger micel be formed, so as to produce asphalitine flocculation and precipitate.
In CO2In oil displacement process, the CO of injection2It is dissolved in crude oil, with CO2Concentration increase in crude oil, it is substantial amounts of CO2Small molecule occupies the space that asphaltene molecules roll into a ball surface, makes the concentration relative reduction of colloid, so causes asphaltene molecules The micella solvated layer that group is formed does not reach certain thickness, or can not form micella.Asphaltene molecules will be further combined with, Bigger micel is formed, so as to produce asphalitine flocculation and precipitate.Also, with the rise of injection pressure, CO2In crude oil Meltage increase, the small molecule component in crude oil also increases as, and the concentration as the colloid of asphalitine stabilizer is further Reduction, asphaltene molecules group is easier to combine to flocculate and precipitate.Fig. 1 is CO2Dissolve in rear asphaltene precipitation process Schematic diagram.In CO2During miscible-phase displacement, CO2Meltage increase in crude oil, so as to cause in the crude oil of mixed phase region Precipitation is more readily formed in asphalitine.
The Quantitative study of asphaltene precipitation.The method of experimental study mainly has the experiment of PVT kettles, static balancing test, light The methods such as credit analysis, frequency image analysing computer.Time-consuming for the experiment of PVT kettles, and the ancient kiln of static balancing test stresses under normal temperature and pressure conditionses, What optical analysis, frequency image analysing computer were obtained is indirect signal, it is impossible to observe the truth of asphalitine, and equipment is extremely Complexity, cost is very high.
The content of the invention
Can clear Real Time Observation crude oil-CO it is an object of the invention to provide one kind2The image of layer, and observable asphalitine From CO2The critical pressure point of the crude oil layer precipitation of saturation, sets up precipitation coating ratio in image and is linearly closed with amount of asphaltene precipitation The dynamic of system determines CO2The method of-crude oil effect generation amount of asphaltene precipitation.
The present invention is directed to the problem of being mentioned in background technology, and the technical scheme taken is:
Dynamic determines CO2The method of-crude oil effect generation amount of asphaltene precipitation:Pass through crude oil piston container using the first ISCO pumps Crude oil is poured into reactor, recycles the 2nd ISCO pumps to pass through CO2Piston container is by CO2Reactor is passed through, and utilizes the 2nd ISCO Pump controls CO2Pressure, pass through CCD camera and computer Real Time Observation crude oil-CO2The image of layer, and use image analysis software The area of asphaltene precipitation and the Size Distribution of particle are determined, a small amount of reservoir is determined by asphaltene deposits amount Indirect Determination Under the conditions of precipitation capacity, the asphaltene deposits image obtained in previous experiments is demarcated by these measured values, set up Coating ratio and amount of asphaltene precipitation linear relationship are precipitated in image.
Said determination method is based on dynamic and determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its structure Microscope including reactor and above reactor, reactor side is connected with CO2Piston container, another side is connected with Crude oil piston container;Microscope is connected with computer.Reactor is in visual high-temperature high-pressure reaction kettle generally cylinder, reactor Portion's cavity is also cylinder, and temperature in use scope is 0 ~ 100 DEG C, and it is 25Mpa that maximum, which bears pressure,.Reactor includes from top to down Visual windows, CO2Layer and crude oil layer, lower section is provided with frosted glass plate and cold light source, for for CO2Saturation oil reservoir provides sufficient light According to.CO2Piston container is connected with the 2nd ISCO pumps;Crude oil piston container is connected with the first ISCO pumps, and the interior pressure of reactor leads to Cross the 2nd ISCO infusions and enter CO2To control, the temperature of reactor is controlled with a high-precision heater.Installed on microscope There is CCD camera, the resolution ratio of image passes through CCD camera and computer Real Time Observation crude oil-CO by operator's control2Layer Image, and the picture photographed can be stored in image processing software, for further handling.
Compared with prior art, the advantage of the invention is that:1)Apparatus of the present invention are simple, with low cost, easy to operate, can Pass through CCD camera and computer Real Time Observation crude oil-CO2The image of layer;2)Under high pressure, it may be clearly seen that in acrylic The asphalitine precipitated on plate, is especially observed that asphalitine from CO2The critical pressure point of the crude oil layer precipitation of saturation;3)Can The area of asphaltene precipitation and the Size Distribution of particle are determined by image analysis software, passes through asphaltene deposits amount indirect determination Method determines the precipitation capacity under a small amount of reservoir conditions, and enters rower to the asphaltene deposits image of acquisition by these measured values It is fixed, set up and coating ratio and amount of asphaltene precipitation linear relationship are precipitated in image.
Brief description of the drawings
Fig. 1 is CO2Dissolve in the schematic diagram of asphaltene precipitation process after crude oil;
Fig. 2 is schematic structural view of the invention;
Fig. 3 is reactor and its supporting structure schematic diagram.
Description of reference numerals:1 the oneth ISCO pumps;2 crude oil piston containers;3 reactors;31 visual windows;32CO2Layer;33 Crude oil layer;34 cold light sources;35 frosted glass;4 CO2Piston container;5 the 2nd ISCO pumps;6 microscopes;7 computers.
Specific embodiment
The present invention program is described further below by embodiment:
Embodiment 1:
Dynamic determines CO2The method of-crude oil effect generation amount of asphaltene precipitation:Held using the first ISCO pumps 1 by crude oil piston Crude oil is poured into reactor 3 by device 2, recycles the 2nd ISCO pumps 5 to pass through CO2Piston container 4 is by CO2Reactor 3 is passed through, and is utilized 2nd ISCO pump 5 control CO2Pressure, pass through CCD camera and computer Real Time Observation crude oil-CO2Layer image, and with scheme The area of asphaltene precipitation and the Size Distribution of particle are determined as analysis software, is determined by asphaltene deposits amount Indirect Determination The precipitation capacity gone out under a small amount of reservoir conditions, is carried out by these measured values to the asphaltene deposits image obtained in previous experiments Demarcation, sets up and coating ratio and amount of asphaltene precipitation linear relationship is precipitated in image.
Said determination method is based on dynamic and determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its structure Microscope 6 including reactor 3 and positioned at the top of reactor 3, the side of reactor 3 is connected with CO2Piston container 4, another side It is connected with crude oil piston container 2;Microscope 6 is connected with computer 7.Reactor 3 is visual high-temperature high-pressure reaction kettle generally cylinder Body, the internal cavity of reactor 3 is also cylinder, and temperature in use scope is 0 ~ 100 DEG C, and it is 25Mpa that maximum, which bears pressure,.Reactor 3 include visual windows 31, CO from top to down2Layer 32 and crude oil layer 33, lower section be provided with frosted glass plate 35 and cold light source 34, for for CO2Saturation oil reservoir provides sufficient illumination.CO2Piston container 4 is connected with the 2nd ISCO pumps 5;Crude oil piston container 2 and first ISCO pumps 1 are connected, and the interior pressure of reactor 3 injects CO by the 2nd ISCO pumps 52To control, the temperature of reactor 3 is high with one The heater control of precision.CCD camera is installed, the resolution ratio of image passes through CCD by operator's control on microscope 6 Camera and computer Real Time Observation crude oil-CO2The image of layer, and the picture photographed can be stored in image processing software, For further handling.
Embodiment 2:
Dynamic determines CO2The method of-crude oil effect generation amount of asphaltene precipitation:Held using the first ISCO pumps 1 by crude oil piston Crude oil is poured into reactor 3 by device 2, recycles the 2nd ISCO pumps 5 to pass through CO2Piston container 4 is by CO2Reactor 3 is passed through, and is utilized 2nd ISCO pump 5 control CO2Pressure, pass through CCD camera and computer Real Time Observation crude oil-CO2Layer image, and with scheme The area of asphaltene precipitation and the Size Distribution of particle are determined as analysis software, is determined by asphaltene deposits amount Indirect Determination The precipitation capacity gone out under a small amount of reservoir conditions, is carried out by these measured values to the asphaltene deposits image obtained in previous experiments Demarcation, sets up and coating ratio and amount of asphaltene precipitation linear relationship is precipitated in image.
Said determination method is based on dynamic and determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its structure Microscope 6 including reactor 3 and positioned at the top of reactor 3, the side of reactor 3 is connected with CO2Piston container 4, another side It is connected with crude oil piston container 2;Microscope 6 is connected with computer 7.Reactor 3 is visual high-temperature high-pressure reaction kettle generally cylinder Body, the internal cavity of reactor 3 is also cylinder, and temperature in use scope is 0 ~ 100 DEG C, and it is 25Mpa that maximum, which bears pressure,.Reactor 3 include visual windows 31, CO from top to down2Layer 32 and crude oil layer 33, lower section be provided with frosted glass plate 35 and cold light source 34, for for CO2Saturation oil reservoir provides sufficient illumination.CO2Piston container 4 is connected with the 2nd ISCO pumps 5;Crude oil piston container 2 and first ISCO pumps 1 are connected, and the interior pressure of reactor 3 injects CO by the 2nd ISCO pumps 52To control, the temperature of reactor 3 is high with one The heater control of precision.CCD camera is installed, the resolution ratio of image passes through CCD by operator's control on microscope 6 Camera and computer Real Time Observation crude oil-CO2The image of layer, and the picture photographed can be stored in image processing software, For further handling.
Every time before experiment, reactor 3 is cleaned with benzene, and is dried up with nitrogen, is then vacuumized.First inject 5MPa CO2Gas Temperature, is set to experimental temperature by body, after pressure stability, and CO is filled using the compression of the 2nd ISCO pumps 52Piston container 4, make Pressure stability is in 9MPa in reactor 3(Higher than crude oil bubble point pressure, crude oil deaeration is prevented).Following programmable first ISCO Pump 1 is by 2.5cm3Crude oil be injected into reactor.The a small amount of crude oil purpose of selection injection is in order to be able to being formed about on form For 0.03cm very thin one layer of oil reservoir, can so light source be set fully to illuminate.Then light crude oil-CO is observed by microscope 62 The image of system layer Crude Oil, passes through CCD camera and computer Real Time Observation crude oil-CO2The image of layer.In this way, Under high pressure, it may be clearly seen that the asphalitine precipitated on acrylic board.It especially can also be observed that asphalitine from CO2It is full The critical pressure point of the crude oil layer precipitation of sum.CO is filled by the compression of the 2nd ISCO pumps 52Piston container 4, make in reactor 3 Pressure is slowly raised next pressure spot, repeats experimentation above.Then asphalitine is determined with image analysis software to sink The area in shallow lake and the Size Distribution of particle.
Embodiment 3:
Dynamic determines CO2The method of-crude oil effect generation amount of asphaltene precipitation:Held using the first ISCO pumps 1 by crude oil piston Crude oil is poured into reactor 3 by device 2, recycles the 2nd ISCO pumps 5 to pass through CO2Piston container 4 is by CO2Reactor 3 is passed through, and is utilized 2nd ISCO pump 5 control CO2Pressure, pass through CCD camera and computer Real Time Observation crude oil-CO2Layer image, and with scheme The area of asphaltene precipitation and the Size Distribution of particle are determined as analysis software, is determined by asphaltene deposits amount Indirect Determination The precipitation capacity gone out under a small amount of reservoir conditions, is carried out by these measured values to the asphaltene deposits image obtained in previous experiments Demarcation, sets up and coating ratio and amount of asphaltene precipitation linear relationship is precipitated in image.
Said determination method is based on dynamic and determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its structure Microscope 6 including reactor 3 and positioned at the top of reactor 3, the side of reactor 3 is connected with CO2Piston container 4, another side It is connected with crude oil piston container 2;Microscope 6 is connected with computer 7.Reactor 3 is visual high-temperature high-pressure reaction kettle generally cylinder Body, the internal cavity of reactor 3 is also cylinder, and temperature in use scope is 0 ~ 100 DEG C, and it is 25Mpa that maximum, which bears pressure,.Reactor 3 include visual windows 31, CO from top to down2Layer 32 and crude oil layer 33, lower section be provided with frosted glass plate 35 and cold light source 34, for for CO2Saturation oil reservoir provides sufficient illumination.CO2Piston container 4 is connected with the 2nd ISCO pumps 5;Crude oil piston container 2 and first ISCO pumps 1 are connected, and the interior pressure of reactor 3 injects CO by the 2nd ISCO pumps 52To control, the temperature of reactor 3 is high with one The heater control of precision.CCD camera is installed, the resolution ratio of image passes through CCD by operator's control on microscope 6 Camera and computer Real Time Observation crude oil-CO2The image of layer, and the picture photographed can be stored in image processing software, For further handling.
The surface of frosted glass plate 3 scribbles clear coat, and its composition and its parts by weight are:10 ~ 20 parts of nano TiO 2s, 15 ~ 30 parts Aqueous polyurethane, 2 ~ 6 parts of absolute ethyl alcohols, 3 ~ 8 parts of n-butanols, 0.02 ~ 0.03 part of levelling agent, 0.8 ~ 1.2 part of defoamer and 0.04 ~ 0.06 part of thickener, 1 ~ 4 part of methanol-functional siloxane resin and 0.6 ~ 1.2 part of polysiloxanes.Methanol-functional siloxane resin Diffusing reflection occurs for the light for sending cold light source by aqueous polyurethane with polysiloxanes, so that uniform light is radiated at reaction In kettle, the error of observation caused by light intensity differs is prevented, while the brightness of light will not be reduced, the waste of the energy is caused.
Every time before experiment, reactor 3 is cleaned with benzene, and is dried up with nitrogen, is then vacuumized.First inject 5MPa CO2Gas Temperature, is set to experimental temperature by body, after pressure stability, and CO is filled using the compression of the 2nd ISCO pumps 52Piston container 4, make Pressure stability is in 9MPa in reactor 3(Higher than crude oil bubble point pressure, crude oil deaeration is prevented).Following programmable first ISCO Pump 1 is by 2.5cm3Crude oil be injected into reactor.The a small amount of crude oil purpose of selection injection is in order to be able to being formed about on form For 0.03cm very thin one layer of oil reservoir, can so light source be set fully to illuminate.Then light crude oil-CO is observed by microscope 62 The image of system layer Crude Oil, passes through CCD camera and computer Real Time Observation crude oil-CO2The image of layer.In this way, Under high pressure, it may be clearly seen that the asphalitine precipitated on acrylic board.It especially can also be observed that asphalitine from CO2It is full The critical pressure point of the crude oil layer precipitation of sum.CO is filled by the compression of the 2nd ISCO pumps 52Piston container 4, make in reactor 3 Pressure is slowly raised next pressure spot, repeats experimentation above.Then asphalitine is determined with image analysis software to sink The area in shallow lake and the Size Distribution of particle.
Routine operation in the operating procedure of the present invention is well known to those skilled in the art, herein without repeating.
Technical scheme is described in detail embodiment described above, it should be understood that it is described above only For the specific embodiment of the present invention, it is not intended to limit the invention, all any modifications made in the spirit of the present invention, Supplement or similar fashion replacement etc., should be included in the scope of the protection.

Claims (8)

1. dynamic determines CO2The method of-crude oil effect generation amount of asphaltene precipitation, it is characterised in that:Utilize the first ISCO pumps(1) Pass through crude oil piston container(2)Crude oil is poured into reactor(3), recycle the 2nd ISCO pumps(5)Pass through CO2Piston container(4) By CO2It is passed through reactor(3), and utilize the 2nd ISCO pumps(5)To control CO2Pressure, it is real-time by CCD camera and computer Observe crude oil-CO2The image of layer, and the area of asphaltene precipitation and the Size Distribution of particle are determined with image analysis software, lead to Cross asphaltene deposits amount Indirect Determination and determine precipitation capacity under a small amount of reservoir conditions, by these measured values to above real The asphaltene deposits image for testing middle acquisition is demarcated, and is set up precipitation coating ratio in image and is linearly closed with amount of asphaltene precipitation System.
2. dynamic according to claim 1 determines CO2The method of-crude oil effect generation amount of asphaltene precipitation, its feature exists In:Described assay method is based on dynamic and determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its structure bag Include reactor(3)With positioned at reactor(3)The microscope of top(6), it is characterised in that:Described reactor(3)Side is connected There is CO2Piston container(4), another side is connected with crude oil piston container(2);Described microscope(6)With computer(7)It is connected.
3. dynamic according to claim 2 determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its feature It is:Described reactor(3)For visual high-temperature high-pressure reaction kettle generally cylinder, reactor(3)Internal cavity is also round Cylinder, temperature in use scope is 0 ~ 100 DEG C, and it is 25Mpa that maximum, which bears pressure,.
4. dynamic according to claim 2 determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its feature It is:Described reactor(3)Include visual windows from top to down(31)、CO2Layer(32)With crude oil layer(33).
5. dynamic according to claim 2 determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its feature It is:Described reactor(3)Lower section is provided with frosted glass plate(35)And cold light source(34).
6. dynamic according to claim 2 determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its feature It is:Described CO2Piston container(4)With the 2nd ISCO pumps(1)It is connected.
7. dynamic according to claim 2 determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its feature It is:Described crude oil piston container(2)With the first ISCO pumps(5)It is connected.
8. dynamic according to claim 2 determines CO2The experimental provision of-crude oil effect generation amount of asphaltene precipitation, its feature It is:Described microscope(6)On CCD camera is installed.
CN201710376823.8A 2017-05-25 2017-05-25 Dynamic determines CO2The method of crude oil effect generation amount of asphaltene precipitation Pending CN107219322A (en)

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Application publication date: 20170929