CN117990665A - In-situ emulsification process description and characterization device, method and system - Google Patents
In-situ emulsification process description and characterization device, method and system Download PDFInfo
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- 238000004945 emulsification Methods 0.000 title claims abstract description 161
- 238000000034 method Methods 0.000 title claims abstract description 78
- 230000008569 process Effects 0.000 title claims abstract description 68
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 52
- 238000012512 characterization method Methods 0.000 title claims abstract description 36
- 238000002347 injection Methods 0.000 claims abstract description 109
- 239000007924 injection Substances 0.000 claims abstract description 109
- 238000004458 analytical method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 76
- 239000000839 emulsion Substances 0.000 claims description 57
- 239000000523 sample Substances 0.000 claims description 37
- 230000000694 effects Effects 0.000 claims description 31
- 239000007850 fluorescent dye Substances 0.000 claims description 11
- 238000011049 filling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000001804 emulsifying effect Effects 0.000 claims description 3
- 238000001215 fluorescent labelling Methods 0.000 claims description 3
- 238000013064 process characterization Methods 0.000 claims 2
- 238000011084 recovery Methods 0.000 abstract description 12
- 230000000007 visual effect Effects 0.000 abstract description 4
- 239000000084 colloidal system Substances 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000004891 communication Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 114
- 239000003921 oil Substances 0.000 description 90
- 238000006073 displacement reaction Methods 0.000 description 7
- 239000008346 aqueous phase Substances 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 4
- 238000003486 chemical etching Methods 0.000 description 3
- 239000010779 crude oil Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- GNBHRKFJIUUOQI-UHFFFAOYSA-N fluorescein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC=C(O)C=C1OC1=CC(O)=CC=C21 GNBHRKFJIUUOQI-UHFFFAOYSA-N 0.000 description 2
- 238000002073 fluorescence micrograph Methods 0.000 description 2
- 238000010191 image analysis Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- VOFUROIFQGPCGE-UHFFFAOYSA-N nile red Chemical compound C1=CC=C2C3=NC4=CC=C(N(CC)CC)C=C4OC3=CC(=O)C2=C1 VOFUROIFQGPCGE-UHFFFAOYSA-N 0.000 description 2
- 239000007764 o/w emulsion Substances 0.000 description 2
- 238000012634 optical imaging Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000004367 cycloalkylaryl group Chemical group 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000799 fluorescence microscopy Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L11/00—Measuring steady or quasi-steady pressure of a fluid or a fluent solid material by means not provided for in group G01L7/00 or G01L9/00
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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- Immunology (AREA)
- Pathology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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- Clinical Laboratory Science (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention provides an in-situ emulsification process description and characterization device, method and system, which belong to the field of oilfield chemistry and colloid interfaces, wherein the device comprises: an injection device; the microfluidic chip is provided with an injection port and an outflow port, a visible micro-channel structure is formed between the injection port and the outflow port, and the micro-channel structure is matched with the channel structure of the core slice; an effluent collector in communication with the effluent outlet; the constant temperature heater is arranged at the bottom of the microfluidic chip; the fluorescence microscope is arranged above the microfluidic chip; the emulsification identification unit is communicated with the fluorescence microscope; the emulsification analysis unit is communicated with the emulsification identification unit; the first pressure sensor is arranged on the sample inlet pipe; and the second pressure sensor is arranged on the outlet pipe. The device provided by the invention can carry out visual research on the in-situ emulsification process, explore the influence of various process variables on the in-situ emulsification, and quantize vermicelli on effluent, thereby being beneficial to improving recovery ratio.
Description
Technical Field
The invention relates to the technical field of oilfield chemistry and colloid interfaces, in particular to an in-situ emulsification process description and characterization device, an in-situ emulsification process description and characterization method and an in-situ emulsification process description and characterization system.
Background
In the field of oil and gas recovery, lowering the oil/water interfacial tension (IFT) to ultra-low levels (< 10 -2mN·m-1) by forming mesophase microemulsions is widely recognized as the primary mechanism by which surfactants enhance recovery. This process generally requires a higher surfactant concentration and the participation of adjuvants. However, the field application of the domestic part of oil fields shows that the recovery ratio can be greatly improved when the surfactant with low concentration is used and the ultra-low IFT is not achieved, for example, the SP compound flooding containing the surfactant cycloalkyl aryl sulfonate (NAS) is used in the Xinjiang oil field, the recovery ratio in the field stage reaches 16%, the final recovery ratio is predicted to reach 20% by numerical simulation, however, the interfacial tension between the system and crude oil is far from reaching the ultra-low level, and the underlying mechanism contained in the system is yet to be revealed.
In recent years, in situ emulsification has been considered as a possible mechanism to enhance recovery. Theoretically, when the poly-surface binary drive flows simultaneously with the crude oil at the pumping pressure, an emulsion is necessarily formed, and the crude oil is necessarily driven to the surface together with the emulsion. Due to its relatively high viscosity, the resulting emulsion helps to block the hypertonic channel, forcing the subsequent displacement fluid to flow towards the hypotonic zone, and thus the residual oil therein. However, due to the complexity of the porous medium geometry and the complexity of the emulsion system, the physical process of emulsion formation and flow is quite complex, how much emulsion is formed in the underground porous medium, how much in situ emulsification affects the recovery efficiency, and how much the polymer affects in situ emulsification, so it is not known at present, and the main reason is that the seepage process in the porous medium cannot be monitored in real time. Thus, the basic mechanism of fluid flow in porous media is visually studied, which is of great importance for understanding the evolution of in situ emulsions and revealing their contribution to enhanced recovery.
Disclosure of Invention
Aiming at the technical problem that in-situ emulsification in the surfactant flooding process is difficult to describe and characterize in the prior art, the invention provides an in-situ emulsification process description and characterization device, an in-situ emulsification process description and characterization method and an in-situ emulsification process description and characterization system.
To achieve the above object, a first aspect of the present invention provides an in-situ emulsification process describing and characterizing device, comprising: the injection device is used for injecting an oil phase or a water phase; the microfluidic chip is provided with an injection port and an outflow port, the injection port of the microfluidic chip is communicated with the injection device, a visible micro-channel structure is formed between the injection port and the outflow port, the micro-channel structure is matched with a channel structure of a core slice, a water phase is injected into the micro-channel structure through the injection port, an oil phase which is injected into the micro-channel structure in advance is emulsified, and emulsion formed after the emulsification or the oil phase which is replaced by the water phase flows out through the outflow port; the effluent collector is communicated with the outflow port of the microfluidic chip and is used for collecting emulsion formed after emulsification or oil phase which is replaced by water phase; the constant temperature heater is arranged at the bottom of the micro-fluidic chip and is used for heating the micro-fluidic chip at constant temperature; the fluorescence microscope is arranged above the micro-fluidic chip and is used for observing the emulsification process of water in the micro-channel structure relative to the oil phase, wherein the oil phase and the water phase are respectively subjected to fluorescence labeling in advance by adopting different fluorescent agents; the emulsification identification unit is communicated with the fluorescence microscope and is used for collecting image information of water relative to oil phase emulsification in the micro-channel structure; the emulsification analysis unit is communicated with the emulsification identification unit and is used for determining the emulsification effect of the water phase and the oil phase based on the image information; the first pressure sensor is arranged on a sample injection pipeline between the injection device and the injection port of the microfluidic chip and is used for detecting the injection pressure of the sample injection pipeline; and the second pressure sensor is arranged on the sample outlet pipe between the injection device and the outflow port of the microfluidic chip and is used for detecting the outflow pressure of the sample outlet pipe.
Further, the injection device includes: the syringe and the micro sample injection pump, the syringe sets up the micro sample injection pump with between the first pressure sensor, the micro sample injection pump is used for adjusting injection volume and injection rate of aqueous phase or oil phase, and through the syringe to advance the injection pipeline pump aqueous phase or oil phase.
Further, the syringe is an airtight syringe.
Further, the apparatus further comprises: the temperature measuring probe is arranged on the surface of the micro-fluidic chip and used for detecting the temperature of the micro-fluidic chip.
Further, the effluent collector is a nuclear magnetic tube.
Further, scale marks for marking standard capacity are arranged on the outer wall of the nuclear magnetic tube.
A second aspect of the present invention provides an in-situ emulsification process description and characterization method applied to the in-situ emulsification process description and characterization apparatus described above, the method comprising: respectively adopting different fluorescent agents to carry out fluorescent marking on the water phase and the oil phase; filling the micro-channel structure of the micro-fluidic chip with an oil phase; injecting a water phase into the micro-channel structure of the micro-fluidic chip, and emulsifying the water phase with respect to the oil phase of the micro-channel structure; collecting image information of water-phase oil phase emulsification of a micro-channel structure; and determining the emulsification effect of water relative to the oil phase based on the image information.
Further, the determining the emulsification effect of water relative to the oil phase based on the image information includes: determining the size and size distribution of the emulsion formed after emulsification based on the image information; the smaller the size of the emulsion formed after emulsification is, the better the emulsification effect is; the more uniform the size distribution of the emulsion formed after emulsification, the better the emulsification effect.
Further, the method further comprises: determining the volume of emulsion formed after emulsification and the volume of oil phase displaced by water phase; the larger the sum of the volume of the emulsion formed after emulsification and the volume of the oil phase displaced by the water phase, the better the emulsification effect.
A third aspect of the invention provides an in situ emulsification process description and characterization system comprising an in situ emulsification process description and characterization device as described above.
Through the technical scheme provided by the invention, the invention has at least the following technical effects:
The in-situ emulsification process description and characterization device comprises an injection device, a microfluidic chip, an effluent collector, a constant temperature heater, a fluorescence microscope, an emulsification identification unit, an emulsification analysis unit and two pressure sensors. The injection device is used for injecting an oil phase or a water phase, the microfluidic chip is provided with an injection port and an outflow port, the injection port of the microfluidic chip is communicated with the injection device, a visible micro-channel structure is formed between the injection port and the outflow port, the micro-channel structure is matched with a channel structure of a core slice, the water phase is injected into the micro-channel structure through the injection port and emulsifies the oil phase which is injected into the micro-channel structure in advance, emulsion formed after emulsification or the oil phase which is replaced by the water phase flows out to an effluent collector through the outflow port, and the constant temperature heater is arranged at the bottom of the microfluidic chip and is used for heating the microfluidic chip at constant temperature. The oil phase and the water phase are respectively subjected to fluorescent marking in advance by adopting different fluorescent agents, and the emulsification process of the water in the micro-channel structure relative to the oil phase can be observed through a fluorescent microscope arranged above the micro-fluidic chip. The emulsification identification unit is communicated with the fluorescence microscope, acquires image information of water relative oil phase emulsification in the micro-channel structure, and transmits the image information to the emulsification analysis unit, and the emulsification analysis unit determines the emulsification effect of water relative oil phase based on the image information. And a first pressure sensor and a second pressure sensor are respectively arranged on a sample injection pipeline between the injection device and the injection port of the microfluidic chip and on a sample outlet pipeline between the injection device and the outflow port of the microfluidic chip and are used for detecting the pressure of the pipeline. The in-situ emulsification process description and characterization device, method and system provided by the invention can simulate an underground porous medium by utilizing a microfluidic chip, carry out visual research on the in-situ emulsification process, explore the influence of various process variables on in-situ emulsification, further analyze the effluent, quantify the effluent and help to improve the recovery ratio.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings are included to provide a further understanding of embodiments of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain, without limitation, the embodiments of the invention. In the drawings:
FIG. 1 is a schematic diagram of an in situ emulsification process description and characterization apparatus provided by an embodiment of the present invention;
Fig. 2 is a schematic diagram of an internal structure of a microfluidic chip in an in-situ emulsification process description and characterization device according to an embodiment of the present invention;
FIG. 3 is a flow chart of an in situ emulsification process description and characterization method provided by an embodiment of the present invention;
FIG. 4 is a schematic illustration of an emulsification process according to one embodiment of the present invention;
FIG. 5 is a schematic illustration of an emulsified emulsion according to one embodiment of the present invention;
FIG. 6 is a graph of the size distribution of an emulsified emulsion according to one embodiment of the present invention;
FIG. 7 is a schematic illustration of an emulsification process according to another embodiment of the present invention;
FIG. 8 is a schematic illustration of an emulsified emulsion according to another embodiment of the present invention;
Fig. 9 is a size distribution diagram of an emulsified emulsion according to another embodiment of the present invention.
Description of the reference numerals
1-A syringe; 2-a microsyringe pump; 3-a first pressure sensor; 4-a second pressure sensor; 5-microfluidic chip; 6-a constant temperature heater; 7-an emulsion analysis unit; 8-an emulsion identification unit; 9-fluorescence microscopy; 10-effluent collector; 11-pressure-resistant clamp.
Detailed Description
The following describes the detailed implementation of the embodiments of the present invention with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
In the present invention, unless otherwise indicated, terms of orientation such as "upper, lower, top, bottom" are used generally with respect to the orientation shown in the drawings or with respect to the positional relationship of the various components with respect to one another in the vertical, vertical or gravitational directions.
The invention will be described in detail below with reference to the drawings in connection with embodiments.
Referring to fig. 1, an embodiment of the present invention provides an in-situ emulsification process description and characterization apparatus, which includes: the injection device is used for injecting an oil phase or a water phase; the microfluidic chip 5 is provided with an injection port and an outflow port, the injection port of the microfluidic chip 5 is communicated with the injection device, a visible micro-channel structure is formed between the injection port and the outflow port, the micro-channel structure is matched with a channel structure of a core slice, a water phase is injected into the micro-channel structure through the injection port, an oil phase which is injected into the micro-channel structure in advance is emulsified, and emulsion formed after the emulsification or the oil phase which is replaced by the water phase flows out through the outflow port; an effluent collector 10, which is communicated with the outflow port of the microfluidic chip 5 and is used for collecting emulsion formed after emulsification or oil phase which is replaced by water phase; the constant temperature heater 6 is arranged at the bottom of the micro-fluidic chip 5 and is used for heating the micro-fluidic chip 5 at constant temperature; the fluorescence microscope 9 is arranged above the micro-fluidic chip 5 and is used for observing the emulsification process of water in the micro-channel structure relative to the oil phase, wherein the oil phase and the water phase are respectively subjected to fluorescence labeling in advance by adopting different fluorescent agents; the emulsification identification unit 8 is communicated with the fluorescence microscope 9 and is used for acquiring image information of the emulsification of water in the micro-channel structure relative to the oil phase; an emulsion analysis unit 7, which is communicated with the emulsion identification unit 8 and is used for determining the emulsion effect of the water phase and the oil phase based on the image information; the first pressure sensor 3 is arranged on a sample injection pipe path between the injection device and the injection port of the microfluidic chip 5 and is used for detecting the injection pressure of the sample injection pipe path; and the second pressure sensor 4 is arranged on the sample outlet pipe path between the injection device and the outflow port of the microfluidic chip 5 and is used for detecting the outflow pressure of the sample outlet pipe path.
In particular, in an embodiment of the present invention, the in situ emulsification process description and characterization device comprises an injection device, a microfluidic chip 5, an effluent collector 10, a fluorescence microscope 9, an emulsification identification unit 8, and an emulsification analysis unit 7. The injection device, the microfluidic chip 5 and the effluent collector 10 are sequentially communicated, and the constant temperature heater 6 is arranged at the bottom of the microfluidic chip 5 and is used for heating the microfluidic chip 5 at constant temperature. Referring to fig. 2, the microfluidic chip 5 has an injection port and an outflow port, the injection port of the microfluidic chip 5 communicates with an injection device, and the outflow port communicates with the effluent collector 10. A visible micro-channel structure is formed between the injection port and the outflow port, the micro-channel structure is matched with the channel structure of the core slice, the core slice can be obtained through real core slice scanning, the water phase is injected into the micro-channel structure through the injection port, the oil phase which is injected into the micro-channel structure in advance is emulsified, and emulsion formed after the emulsification or the oil phase which is replaced by the water phase flows out through the outflow port and is collected in the effluent collector 10. In one possible embodiment, the microfluidic chip 5 is made of glass, and the micro-channel structure is formed on the glass substrate through plate making, coating, optical imaging, chemical etching, sintering, wetting, and the like, and two holes are drilled at two diagonal ends of the microfluidic chip 5 as an injection port and an outflow port, respectively. The average depth of the microchannel structure was 100 μm and the cross-sectional area was 4.2mm 2, the porosity was about 44.3% by image analysis and the permeability was about 8.8Darcy by water injection.
The fluorescence microscope 9 is arranged above the microfluidic chip 5, can distinguish oil/water two phases under the fluorescence excitation condition, and observes the emulsification process of water relative to oil phase in the micro-channel structure. The emulsification identification unit 8 is communicated with the fluorescence microscope 9, can acquire image information of water-to-oil phase emulsification in the micro-channel structure, and sends the image information to the emulsification analysis unit 7, and the emulsification analysis unit 7 determines the emulsification effect of water-to-oil phase based on the image information. A first pressure sensor 3 is arranged on a sample injection pipeline between the injection device and the injection port of the microfluidic chip 5, and can detect the injection pressure of the sample injection pipeline. A second pressure sensor 4 is provided on the outlet pipe between the injection device and the outflow port of the microfluidic chip 5, and can detect the outflow pressure of the sample pipe. The detection limit of the first pressure sensor 3 and the second pressure sensor 4 is 800kPa. In one possible embodiment, the fluorescence microscope 9 is connected to the stage by a bracket, the microfluidic chip 5 and the constant temperature heater 6 are placed on the stage, and the fluorescence microscope 9 is disposed above the microchannel structure. The fluorescence microscope 9 contains three excitation modes of blue, green and red fields. The emulsion recognition unit 8 employs a high-speed camera whose maximum photographing rate in the full-frame width mode is 2000 frames/second.
According to the in-situ emulsification process description and characterization device provided by the invention, the micro-fluidic chip can be used for simulating an underground porous medium, the in-situ emulsification process can be subjected to visual research, the influence of various process variables on in-situ emulsification is explored, the effluent can be further analyzed, the effluent is quantized, and the recovery ratio is improved.
Further, the injection device includes: the injection device comprises an injector 1 and a microsyringe pump 2, wherein the injector 1 is arranged between the microsyringe pump 2 and the first pressure sensor 3, and the microsyringe pump 2 is used for adjusting the injection amount and the injection speed of an aqueous phase or an oil phase and pumping the aqueous phase or the oil phase into the sampling pipeline through the injector 1.
Specifically, in the embodiment of the invention, the injection device comprises the injector 1 and the micro sample injection pump 2, the injector 1 is arranged between the micro sample injection pump 2 and the first pressure sensor 3, the micro sample injection pump 2 can adjust the injection amount and the injection speed of the water phase or the oil phase, and the water phase or the oil phase is pumped into the sample injection pipeline through the injector 1. In one possible embodiment, the syringe 1 is a gas-tight syringe.
Further, the apparatus further comprises: the temperature measuring probe is arranged on the surface of the micro-fluidic chip 5 and is used for detecting the temperature of the micro-fluidic chip 5.
Specifically, in the embodiment of the present invention, a temperature probe is disposed on the surface of the microfluidic chip 5, and the temperature probe can detect the temperature of the microfluidic chip 5 in real time, so as to ensure that the constant temperature heater 6 controls the microfluidic chip 5 within a suitable temperature range (for example, around 60 ℃).
Further, the effluent collector 10 is a nuclear magnetic resonance tube.
Further, scale marks for marking standard capacity are arranged on the outer wall of the nuclear magnetic tube.
Specifically, in the embodiment of the invention, the effluent liquid collector 10 is a nuclear magnetic tube, the outer wall of the nuclear magnetic tube is provided with scale marks for marking standard capacity, and staff can intuitively obtain the volume of emulsion formed after emulsification and the volume of oil phase driven out by water phase according to the scale marks, so that the emulsification effect can be conveniently represented.
Further, the apparatus further comprises: the pressure-resistant clamp 11 is of a sheet structure with square through holes, the square through holes of the pressure-resistant clamp 11 expose the visible micro-channel structure, the injection port and the outflow port of the micro-fluidic chip 5, are pressed on four sides of the micro-fluidic chip 5, and are fixed with the constant temperature heater 6.
Specifically, in the embodiment of the invention, the pressure-resistant clamp 11 is arranged on the microfluidic chip 5, a square through hole is arranged in the middle of the pressure-resistant clamp 11, the pressure-resistant clamp 11 is pressed on four sides of the microfluidic chip 5 and is fixed with the constant temperature heater 6, and the square through hole of the pressure-resistant clamp 11 exposes the visible micro-channel structure, the injection port and the outflow port of the microfluidic chip 5. The pressure-resistant clamp 11 can prevent the micro-fluidic chip 5 from shifting in the observation process, and ensure the stability of the device. The microfluidic chip 5 can bear the injection pressure of 3MPa at maximum after being additionally provided with the pressure-resistant clamp 11.
Referring to fig. 3, a second aspect of the present invention provides an in-situ emulsification process description and characterization method applied to the in-situ emulsification process description and characterization apparatus described above, the method comprising the steps of: s101: respectively adopting different fluorescent agents to carry out fluorescent marking on the water phase and the oil phase; s102: filling the micro-channel structure of the micro-fluidic chip with an oil phase; s103: injecting a water phase into the micro-channel structure of the micro-fluidic chip, and emulsifying the water phase with respect to the oil phase of the micro-channel structure; s104: collecting image information of water-phase oil phase emulsification of a micro-channel structure; s105: and determining the emulsification effect of water relative to the oil phase based on the image information.
Specifically, in the embodiment of the invention, firstly, different fluorescent agents are adopted to carry out fluorescent marking on the water phase and the oil phase, the micro-sample injection pump 2 is respectively injected, firstly, the micro-sample injection pump 2 is used for filling the oil phase into the micro-fluidic chip 5, so that the micro-channel structure of the micro-fluidic chip 5 is filled with the oil phase, then, the micro-sample injection pump 2 is used for filling the micro-channel structure of the micro-fluidic chip 5 with the water phase made of the surfactant, the oil phase which is injected into the micro-channel structure in advance is emulsified, a worker can acquire image information of the emulsification process of water in the micro-channel structure relative to the oil phase through the fluorescent microscope 9 and the emulsification identification unit 8, and the emulsification analysis unit 7 is used for determining the emulsification effect of the water relative to the oil phase based on the image information. The emulsion formed after emulsification or the oil phase displaced by the water phase flows out through the outflow port and is collected into the effluent collector 10, and a worker can determine the emulsification effect of the water phase relative to the oil phase according to the volume of the emulsion formed after emulsification in the effluent collector 10 and the volume of the oil phase displaced by the water phase. In the emulsification process, the injection pressure of the sample injection pipeline and the outflow pressure of the sample outlet pipeline can be monitored through the first pressure sensor 3 and the second pressure sensor 4, and meanwhile, the pressure change in the emulsification process can be reflected through the injection pressure and the outflow pressure, so that whether the water phase acts on the oil phase or not is reflected.
According to the in-situ emulsification process description and characterization device provided by the invention, the micro-fluidic chip can be used for simulating an underground porous medium, the in-situ emulsification process can be subjected to visual research, the influence of various process variables on in-situ emulsification is explored, the effluent can be further analyzed, the effluent is quantized, and the recovery ratio is improved.
Further, the determining the emulsification effect of water relative to the oil phase based on the image information includes: determining the size and size distribution of the emulsion formed after emulsification based on the image information; the smaller the size of the emulsion formed after emulsification is, the better the emulsification effect is; the more uniform the size distribution of the emulsion formed after emulsification, the better the emulsification effect.
Specifically, in the embodiment of the invention, the emulsification effect can be determined according to the size and the size distribution of the emulsion formed after emulsification, and the smaller the size of the emulsion formed after emulsification is, the better the emulsification effect is, the more uniform the size distribution of the emulsion formed after emulsification is, and the better the emulsification effect is.
Further, the method further comprises: determining the volume of emulsion formed after emulsification and the volume of oil phase displaced by water phase; the larger the sum of the volume of the emulsion formed after emulsification and the volume of the oil phase displaced by the water phase, the better the emulsification effect.
Specifically, in the embodiment of the invention, the emulsification effect can be determined according to the volume of the emulsion formed after emulsification and the volume of the oil phase displaced by the water phase. The larger the sum of the volume of the emulsion formed after emulsification and the volume of the oil phase displaced by the water phase, the better the emulsification effect. The larger the emulsion volume is, the better the emulsification effect is, and the larger the oil phase volume is, the better the oil displacement effect is.
Example 1
The microfluidic chip 5 having a random microchannel structure was prepared by chemical etching. Fig. 2 is a schematic plan view of a pore structure of a chip. The preparation method comprises the steps of plate making, coating, optical imaging, chemical etching, sintering and wetting. The micro-channel structure was etched on a 64mm×64mm glass substrate, the size of the micro-channel structure was 42mm×42mm, and two holes were drilled at both ends of the diagonal line of the mold as an injection port and an outflow port, respectively. The average depth of the microchannel structure was 100 μm and the cross-sectional area was 4.2mm 2, the porosity was about 44.3% by image analysis and the permeability was about 8.8Darcy by water injection.
After the pipe connection, the microfluidic chip 5 was horizontally fixed on a constant temperature heater at 40 ℃, and white oil was pumped into the microfluidic chip 5 at a high injection rate (100 μl·min -1) to ensure saturation of the channel with oil. After the oil saturation process is finished, sodium dodecyl benzene sulfonate aqueous solution with the mass fraction of 1.6% is injected into the channel at a certain rate for emulsification, the real-time pressure is recorded, and the temperature and the injection flow are monitored at the same time, so that the consistency of different experimental groups is ensured. The emulsification process was carried out using a 2.5ml air-tight syringe with an injection rate of 10. Mu.l.min -1.
To distinguish the oil and water phases, the aqueous phase was labeled with 1X 10 -4mol·L-1 fluorescein and the oil phase was labeled with 3X 10 -5mol·L-1 nile red. The emulsification process was imaged using a fluorescence microscope, and fluorescent images were captured using an excitation filter with a wavelength range of 420-485 nm and an emission filter with a wavelength of 515 nm.
The emulsion generation was recorded using a high-speed camera. Fig. 4 shows an emulsification process with 1.6% aqueous sodium dodecylbenzenesulfonate as the injection fluid in a microfluidic chip. Within the dashed box is the exact location where emulsification occurs, and the inset shows the evolution of emulsification over time. It can be seen from the figure that when the residual oil reaches the pore throat (at this point of initiation), the residual oil front is gradually squeezed within 50-170ms due to the displacement pressure being less than capillary resistance, eventually "biting" (Snapping action) at 200ms, but there is still a significant amount of tail residual oil retained in the throat, and from the 240ms captured image, the separated residual oil quickly becomes spherical, forming pore throat sized emulsion droplets and migrating downstream.
Referring to fig. 5, after emulsification for 1 hour, the emulsification conditions in the microfluidic chip 5 were collected, and the emulsion size was counted by Digimizer software, and referring to table 1, the obtained data were shown as a size distribution chart in fig. 6, and the average size of the emulsion in this example was 117 μl and the standard deviation was 40 μl. During displacement effluent was collected and the volume of each phase was measured, in this example 296 μl of oil phase was collected together and 63 μl of oil-in-water emulsion was collected.
TABLE 1
| Size of the device | Quantity of | Intermediate value | Standard deviation of | Minimum value | Maximum value |
| Length of | 104 | 116.9577μl | 40.4950μl | 42.820μl | 253.254μl |
Example two
The microfluidic chip used in this implementation remained identical to the chip in embodiment one. After the pipe connection, the microfluidic chip 5 was fixed horizontally on a 40 ℃ heat table, and white oil was pumped into the microfluidic chip 5 at a high injection rate (100 μl·min -1) to ensure that the channels were saturated with oil. After the oil saturation process is finished, sodium dodecyl benzene sulfonate aqueous solution with mass fraction of 0.2% is injected into the channel at a certain rate for emulsification, real-time pressure is recorded, and meanwhile, the temperature and the injection flow are monitored to ensure the consistency of different experimental groups. The emulsification process was carried out using a 2.5ml air-tight syringe with an injection rate of 10. Mu.l.min -1.
To distinguish the oil and water phases, the aqueous phase was labeled with 1X 10 -4mol·L-1 fluorescein and the oil phase was labeled with 3X 10 -5mol·L-1 nile red. The displacement process was imaged with a fluorescence microscope, and fluorescence images were captured using an excitation filter with a wavelength range of 420-485 nm and an emission filter with a wavelength of 515 nm.
The emulsion generation was recorded using a high-speed camera. Fig. 7 shows an emulsification process with 0.2% aqueous sodium dodecylbenzenesulfonate as the injection fluid in a microfluidic chip. With the present embodiment, since the interfacial tension is high (2.3 mn·m -1), the capillary resistance is high, and the oil cake is hardly emulsified into small droplets through a narrow pore throat (as indicated by white arrows in fig. 7), but can pass through a larger pore throat to be divided into large-sized droplets. As shown by the dashed box and inset in fig. 7, when the residual oil reaches the large-size orifice throat (0 ms), the leading edge of the cake is gradually squeezed and deformed within 40-110 ms and finally divided at 140ms, and the separated oil becomes spherical under the action of interfacial tension, forming emulsion droplets matching the orifice throat size.
Referring to FIG. 8, after 1 hour of displacement, the emulsion in the chip was photographed, and the droplet size was counted using Digimizer software, and the obtained data was used as a size distribution chart as shown in FIG. 9, in this example, the average size of the emulsion was 146. Mu.m, and the standard deviation was 72. Mu.m. During displacement, effluent was collected and the volume of each phase was measured, in this example 294 μl of oil phase was collected together, 50 μl of oil-in-water emulsion.
A third aspect of the invention provides an in situ emulsification process description and characterization system comprising an in situ emulsification process description and characterization device as described above.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (10)
1. An in situ emulsification process characterization device, the device comprising:
the injection device is used for injecting an oil phase or a water phase;
the microfluidic chip (5), the said microfluidic chip (5) has injection port and outflow port, the injection port of the said microfluidic chip (5) communicates with said injection device, there is visible microchannel structure between said injection port and said outflow port, the said microchannel structure matches with channel structure of the core slice, the water phase is injected into the said microchannel structure through the said injection port, and emulsify the oil phase injected into the said microchannel structure in advance, emulsion formed after emulsification or oil phase driven out by the water phase flows out through the said outflow port;
the effluent collector (10) is communicated with the outflow port of the microfluidic chip (5) and is used for collecting emulsion formed after emulsification or oil phase which is replaced by water phase;
The constant temperature heater (6) is arranged at the bottom of the micro-fluidic chip (5) and is used for heating the micro-fluidic chip (5) at constant temperature;
The fluorescence microscope (9) is arranged above the micro-fluidic chip (5) and is used for observing the emulsification process of water in the micro-channel structure relative to an oil phase, wherein the oil phase and the water phase are respectively subjected to fluorescence labeling in advance by adopting different fluorescent agents;
The emulsification identification unit (8) is communicated with the fluorescence microscope (9) and is used for collecting image information of water relative to oil phase emulsification in the micro-channel structure;
An emulsification analysis unit (7) communicated with the emulsification identification unit (8) and used for determining the emulsification effect of the water phase and the oil phase based on the image information;
The first pressure sensor (3) is arranged on a sample injection pipeline between the injection device and the injection port of the microfluidic chip (5) and is used for detecting the injection pressure of the sample injection pipeline;
and the second pressure sensor (4) is arranged on the sample outlet pipe between the injection device and the outflow port of the microfluidic chip (5) and is used for detecting the outflow pressure of the sample outlet pipe.
2. The in situ emulsification process characterization device of claim 1, wherein the injection device comprises:
The syringe (1) and micro sample injection pump (2), syringe (1) set up micro sample injection pump (2) with between first pressure sensor (3), micro sample injection pump (2) are used for adjusting injection volume and injection rate of water phase or oil phase, and through syringe (1) to advance the injection pipeline pump water phase or oil phase.
3. The in situ emulsification process description and characterization device according to claim 2, characterized in that the syringe (1) is a gas tight syringe.
4. The in situ emulsification process description and characterization device of claim 1, wherein the device further comprises:
The temperature measuring probe is arranged on the surface of the micro-fluidic chip (5) and is used for detecting the temperature of the micro-fluidic chip (5).
5. The in situ emulsification process description and characterization device of claim 1, characterized in that the effluent collector (10) is a nuclear magnetic tube.
6. The in-situ emulsification process description and characterization device according to claim 5, wherein graduation lines for identifying standard capacity are provided on the outer wall of the nuclear magnetic tube.
7. An in situ emulsification process description and characterization method, characterized in that the method is applied to an in situ emulsification process description and characterization device according to any one of the claims 1-6, the method comprising:
Respectively adopting different fluorescent agents to carry out fluorescent marking on the water phase and the oil phase;
filling the micro-channel structure of the micro-fluidic chip with an oil phase;
injecting a water phase into the micro-channel structure of the micro-fluidic chip, and emulsifying the water phase with respect to the oil phase of the micro-channel structure;
Collecting image information of water-phase oil phase emulsification of a micro-channel structure;
and determining the emulsification effect of water relative to the oil phase based on the image information.
8. The in situ emulsification process description and characterization method of claim 7 wherein the determining the emulsification effect of water relative to oil phase based on the image information comprises:
Determining the size and size distribution of the emulsion formed after emulsification based on the image information;
the smaller the size of the emulsion formed after emulsification is, the better the emulsification effect is;
the more uniform the size distribution of the emulsion formed after emulsification, the better the emulsification effect.
9. The in situ emulsification process description and characterization method of claim 7, further comprising:
determining the volume of emulsion formed after emulsification and the volume of oil phase displaced by water phase;
The larger the sum of the volume of the emulsion formed after emulsification and the volume of the oil phase displaced by the water phase, the better the emulsification effect.
10. An in situ emulsification process description and characterization system comprising the in situ emulsification process description and characterization device of any one of claims 1 to 6.
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| PCT/CN2023/140741 WO2024088443A1 (en) | 2022-10-27 | 2023-12-21 | In-situ emulsification process description and characterization apparatus, method and system |
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