A multifunctional integrated experimental device for preparing and simultaneously measuring emulsion properties and its working method

Abstract

The present invention relates to a multifunctional integrated experimental device for preparing and simultaneously measuring emulsion properties, and its operating method. The device comprises a fluid injection system, an emulsion generation system, an emulsion testing system, and a produced fluid collection system. During the experiment, the aqueous phase and oil phase are pumped into the emulsion generation system via the fluid injection system. After the emulsion is generated, it enters the emulsion testing system through a six-way valve, where its phase state, viscosity, and stability are simultaneously measured. Finally, the produced fluid collection system collects and processes the emulsion. The present invention achieves the generation of emulsions in porous core media under high-pressure experimental conditions and the simultaneous measurement of their phase state, viscosity, and stability. This device can provide a multifunctional integrated experimental device for further studying the generation and evolution characteristics of emulsions in porous media.

Description

Technical Field

[0001] The invention relates to a multifunctional integrated experimental device for preparing emulsion and synchronously measuring its characteristics and a working method thereof, belonging to the technical field of oil and gas field development. Background Art

[0002] my country has vast heavy oil reserves, but current development primarily relies on water flooding and steam stimulation, resulting in relatively low overall recovery rates. Furthermore, heavy oil thermal recovery is often plagued by high emissions, high costs, and poor returns. As my country implements its "dual carbon" strategy, chemical composite cold recovery technology has emerged as a promising technology for reducing emissions and increasing production in heavy oil reservoirs with multiple cycles of stimulation and inefficient water flooding.

[0003] Emulsification is the primary mechanism for enhancing crude oil recovery in heavy oil chemical composite cold recovery technology. Specifically, by injecting an aqueous solution containing an emulsifier and stabilizer into a heavy oil reservoir, the highly viscous heavy oil is emulsified in situ within the porous medium to form an emulsion, thereby facilitating the displacement of the difficult-to-move heavy oil. The phase state, viscosity, and stability of the emulsion significantly influence its flow in porous media. Therefore, it is essential to prepare a variety of emulsions in the laboratory under different conditions and to conduct in-depth research on their properties, such as phase state, viscosity, and stability.

[0004] Currently, laboratories mostly use membrane emulsification, high-speed stirring, ultrasonic emulsification, and microfluidics to prepare emulsions. The prepared emulsions are then transferred to different analytical instruments for separate property measurements. Membrane emulsification has poor operability and is expensive, while high-speed stirring and ultrasonic emulsification require high equipment requirements, high energy consumption, and demanding preparation conditions. Microfluidics is limited by chip technology and has low preparation efficiency. Furthermore, by first generating the emulsion and then transferring it to different instruments for separate property measurements, it is difficult to ensure the timeliness and comparability of the measurement results. Summary of the Invention

[0005] In response to the shortcomings of the existing technology, the present invention proposes a multifunctional integrated experimental device for emulsion preparation and simultaneous measurement of properties, which simultaneously realizes the in-situ emulsification of heavy oil inside porous media and the measurement of emulsion phase, viscosity and stability. It is used to meet the needs of experimental devices for the generation and simultaneous measurement of properties of emulsions during heavy oil emulsification production, provides a reliable experimental device for in-depth research on the seepage characteristics of emulsions, and is conducive to the promotion and implementation of heavy oil chemical composite cold production technology, thereby effectively reducing heat energy consumption and emissions of harmful gases such as carbon dioxide.

[0006] The present invention also provides a working method of the multifunctional integrated experimental device for preparing the emulsion and simultaneously measuring its properties.

[0007] Explanation of terms:

[0008] Phase state of emulsion: refers to the morphology or type of emulsion, which generally includes oil-in-water type and water-in-oil type. Oil-in-water emulsion refers to a dispersion system formed by the oil phase dispersed in the form of discrete droplets in a continuous water phase that is immiscible with it, and water-in-oil emulsion refers to a dispersion system formed by the water phase dispersed in the form of discrete droplets in a continuous oil phase that is immiscible with it.

[0009] Viscosity: It is a measure of the fluid's resistance to shear. The viscosity of an emulsion determines its flow capacity in an oil reservoir, and its size is related to factors such as the oil-water volume ratio and the size of discrete droplets.

[0010] Stability: refers to the ability of discrete droplets to resist coalescence, avoid separation of oil and water phases, and even emulsion demulsification and stratification.

[0011] The technical solution of the present invention is:

[0012] A multifunctional integrated experimental device for preparing and simultaneously measuring emulsion properties, comprising a fluid injection system, an emulsion generation system, an emulsion testing system, and a produced fluid collection system;

[0013] During the experiment, the water phase and oil phase were pumped into the emulsion generation system through the fluid injection system. After the emulsion was generated, it entered the emulsion testing system, where the phase state, viscosity and stability of the emulsion were simultaneously measured. Finally, the emulsion was collected and processed by the production fluid collection system.

[0014] According to the preferred embodiment of the present invention, the fluid injection system includes a micro-injection pump, a temperature-resistant and pressure-resistant intermediate container, and a flow regulator connected in sequence; the temperature-resistant and pressure-resistant intermediate container includes a temperature-resistant and pressure-resistant intermediate container for storing a water phase and a temperature-resistant and pressure-resistant intermediate container for storing an oil phase;

[0015] A micro-injection pump pumps distilled water into and drives the pistons in the temperature-resistant and pressure-resistant intermediate container for storing the water phase and the temperature-resistant and pressure-resistant intermediate container for storing the oil phase; a flow controller adjusts the mixing ratio of the water phase and the oil phase to simulate the emulsification of heavy oil in the reservoir under different water content conditions.

[0016] According to a preferred embodiment of the present invention, the emulsion generation system includes a digital pressure controller, a nested micro-injector, a core holder, an artificial core model, and a confining pressure device; the outlet end of the nested micro-injector is connected to the inlet end of the core holder and the digital pressure controller, the artificial core model is placed in the core holder, and the core holder is connected to the confining pressure device;

[0017] Among them, the digital pressure controller is used to collect the injection pressure during the emulsion formation and seepage process, the artificial core model is used to simulate the formation of emulsion in porous media, and the confining pressure device is used to control the pressure state inside the artificial core model.

[0018] Further preferably, the artificial core model is a cylinder.

[0019] Further preferably, the nested micro-injector is composed of an inner tube and an outer tube nested together, the inner tube is embedded in the outer tube, and the inner and outer tubes are axially parallel and fixed; the tail of the nested micro-injector is a conical collection port. During the experiment, the water phase is pumped in from the outer tube and the oil phase is pumped in from the inner tube. The water phase and the oil phase are pumped into the artificial core model through the conical collection port in a coaxial fluid focusing manner.

[0020] According to the preferred embodiment of the present invention, the emulsion testing system includes a phase determination device, a viscosity measurement device and a stability analysis device;

[0021] The phase determination device is used to measure the phase state of the emulsion; the viscosity measuring device is used to measure the viscosity of the emulsion; and the stability analysis device is used to measure the stability of the emulsion.

[0022] According to a preferred embodiment of the present invention, the phase determination device includes a syringe-type droplet ejector, a hydrophilic ceramic plate, a visual glass observation window, and an adjustable distance bracket; the hydrophilic ceramic plate is perpendicular to the outlet end of the syringe-type droplet ejector;

[0023] The syringe-type droplet ejector sprays the emulsion in the form of droplets onto the hydrophilic ceramic plate; the hydrophilic ceramic plate controls the occurrence form of the different phases of the emulsion sprayed onto the hydrophilic ceramic plate through its surface hydrophilic properties;

[0024] The visual glass observation window is used to microscopically observe the occurrence morphology of the emulsion on the surface of the hydrophilic ceramic plate;

[0025] The adjustable distance bracket controls the distance between the hydrophilic ceramic plate and the outlet end of the syringe-type droplet ejector by rotating the screw;

[0026] Further preferably, the phase determination device further comprises a microscope, a high-speed camera and a computer;

[0027] The microscope is installed just above the hydrophilic ceramic plate and is connected to a high-speed camera and a computer to determine the phase state of the generated emulsion.

[0028] Further preferably, the syringe-type droplet ejector comprises an inlet conduit, a cap, a fixed steel sleeve, a sealing ring, a telescopic controller, a flexible hinge displacement groove, a fluid chamber, a telescopic plate, a one-way valve, a necking hole, an outlet conduit and a microfluidic control sheet;

[0029] A cap is provided on the left side of the fluid chamber, and fixed steel sleeves are provided on the upper and lower sides of the fluid chamber. The space formed by the cap and the fixed steel sleeve is the fluid chamber; a flexible hinge displacement groove and a sealing ring are provided in sequence below the fixed steel sleeve on the upper side of the fluid chamber; a flexible hinge displacement groove and a sealing ring are provided in sequence above the fixed steel sleeve on the lower side of the fluid chamber; a telescopic plate is provided longitudinally within the fluid chamber, dividing the fluid chamber into a fluid chamber at the front end of the telescopic plate and a fluid chamber at the rear end of the telescopic plate, and a one-way valve is provided on the telescopic plate; a necking hole, an outlet conduit and a microfluidic control plate are provided in sequence on the right side of the fluid chamber; and micropores are provided on the microfluidic control plate.

[0030] During the experiment, the emulsion enters the fluid chamber at the front end of the telescopic plate through the inlet duct and enters the fluid chamber at the rear end of the telescopic plate through the one-way valve. The telescopic controller controls the telescopic plate to move rapidly along the flexible hinge displacement groove toward the outlet duct, thereby generating a rapid pressurization effect on the fluid chamber at the rear end of the telescopic plate, pushing the emulsion into the outlet duct through the necking hole and finally ejecting it from the micropores on the microfluidic control plate at the end of the outlet duct. After each ejection is completed, the telescopic controller controls the telescopic plate to move slowly along the flexible hinge displacement groove toward the inlet duct, prompting the emulsion in the fluid chamber at the front end of the telescopic plate to enter the fluid chamber at the rear end of the telescopic plate through the one-way valve again, and repeating the above ejection process.

[0031] Further preferably, the cover cap and the fixed steel sleeve are made of 303 stainless steel.

[0032] According to a preferred embodiment of the present invention, the viscosity measuring device includes a capillary bundle model, a measuring cylinder, and a micro differential pressure gauge; wherein the inlet end of the capillary bundle model is connected to the emulsion input pipeline, the outlet end of the capillary bundle model is connected to the measuring cylinder, and the micro differential pressure gauge is connected to the inlet end and the outlet end of the capillary bundle model respectively;

[0033] During the experiment, the volume of the emulsion flowing through the capillary bundle model per unit time was collected using a graduated cylinder, and the pressure difference at both ends of the capillary bundle model was measured using a micro-differential pressure meter. Based on this, the viscosity of the emulsion was calculated.

[0034] According to the preferred embodiment of the present invention, the stability analysis device includes a conductivity meter, a graduated glass liquid collecting tube, a conductivity probe, and a conductivity analysis system;

[0035] The conductivity probe of the conductivity meter is placed at the bottom of a graduated glass collecting tube and connected to a conductivity analysis system. The conductivity analysis system collects the conductivity signal of the emulsion in real time and analyzes the conductivity changes.

[0036] During the experiment, electrodes installed at different positions on the conductivity probe accurately measure the liquid conductivity signal at that position and transmit it to the conductivity analysis system through wires. At the same time, a conductivity value change curve at different times and positions is plotted. If the conductivity values ​​at different times and positions are constant, it indicates that the emulsion is relatively stable. If the conductivity value at the upper end of the graduated glass collecting tube decreases and the conductivity value at the lower end increases within a certain period of time, it indicates that the emulsion has broken and stratified, and its stability is poor.

[0037] Preferably, according to the present invention, the produced fluid collection system is a produced fluid collection device for collecting the remaining emulsion during the experiment.

[0038] The working method of the multifunctional integrated experimental device for preparing and simultaneously measuring the properties of the emulsion includes:

[0039] The water phase and oil phase are pumped into the emulsion generation system through the fluid injection system; after the emulsion is generated in the emulsion generation system, it enters the emulsion testing system, where the phase state, viscosity and stability of the emulsion are simultaneously measured, and finally the produced fluid collection system collects and processes it.

[0040] The working method of the multifunctional integrated experimental device for preparing emulsions and simultaneously measuring their properties comprises the following specific steps:

[0041] (1) The aqueous solution formed by dissolving the emulsifier and stabilizer in the formation water is stored in a temperature-resistant and pressure-resistant intermediate container as the experimental water phase, and the crude oil produced from the actual oil reservoir is dehydrated and stored in a temperature-resistant and pressure-resistant intermediate container as the experimental oil phase; the injection rate of the water phase and the oil phase is regulated by a micro-injection pump and a flow controller, and the back pressure in the experiment is set by a confining pressure device;

[0042] (2) injecting the oil phase and the water phase into the artificial core model through the inner tube and outer tube of the nested microinjector respectively to generate an emulsion, which flows into the six-way valve through the outlet of the artificial core model and enters the emulsion testing system;

[0043] (3) In the phase determination experiment, the emulsion enters the syringe droplet ejector through the six-way valve. The adjustable distance bracket between the hydrophilic ceramic plate and the syringe droplet ejector is adjusted so that the emulsion is deposited on the hydrophilic ceramic plate after passing through the microfluidic control plate. The state of the emulsion in the visual glass observation window is observed by a microscope and a high-speed camera. If the emulsion forms liquid droplets on the hydrophilic ceramic plate, it is an oil-in-water emulsion. If the emulsion forms a thin emulsion film on the hydrophilic ceramic plate, it is an oil-in-water emulsion. The emulsion state is stored by a computer.

[0044] In the viscosity measurement experiment, the emulsion enters the inlet of the capillary bundle model through a six-way valve, flows through the capillary bundle model, and enters the graduated cylinder at the outlet for collection. The volume of the emulsion flowing through the capillary bundle model per unit time is measured. At the same time, a micro-differential pressure gauge is used to measure the pressure difference between the two ends of the capillary bundle model during the emulsion flow. Based on this, the viscosity of the emulsion is calculated.

[0045] In the stability analysis experiment, the emulsion enters a graduated glass manifold through a six-way valve. Electrodes installed at different locations on the conductivity probe accurately measure the liquid conductivity signal at that location and transmit it to the conductivity analysis system via wires. A curve of conductivity values ​​at different times and locations is simultaneously plotted. If the conductivity values ​​remain constant at different times and locations, the emulsion is considered stable. If the conductivity value at the upper end of the graduated glass manifold decreases while the conductivity value at the lower end increases over a certain period of time, the emulsion is experiencing demulsification and separation, indicating poor stability.

[0046] The excess emulsion generated during the experiment enters the produced fluid collection device through a six-way valve for collection and treatment.

[0047] According to the preferred embodiment of the present invention, the viscosity of the emulsion is calculated as shown in formula (I):

[0048]

[0049] In formula (I), η represents the viscosity of the emulsion, Q represents the volume of the emulsion flowing through the capillary bundle model per unit time, ΔP represents the pressure difference across the capillary bundle model, n represents the number of parallel capillaries arranged in the capillary bundle model, r represents the radius of each capillary, and L represents the length of each capillary.

[0050] The beneficial effects of the present invention are:

[0051] 1. The present invention uses a flow controller, a nested micro-injector, an artificial core model, and a confining pressure device to achieve in-situ generation of emulsions inside porous media under different pore throat structures, different oil-water ratios, different pressures, and different hydrodynamic conditions. This effectively covers the diversity of emulsion generation during chemical composite cold recovery in real oil reservoirs and ensures the broad representativeness of the experimental results.

[0052] 2. The present invention avoids mutual interference among emulsion property measurements by simultaneously measuring emulsion formation and its phase state, viscosity and stability, and ensures that the above three property measurement results belong to exactly the same emulsion generated under the same conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0053] Figure 1 A schematic diagram of a multifunctional integrated experimental device for simultaneous preparation and characterization of emulsions;

[0054] Figure 2 Schematic diagram of the nested microinjector structure;

[0055] Figure 3 Schematic diagram of the structure of a syringe-type droplet ejector;

[0056] Figure 4 This is a micrograph of the emulsion's storage state;

[0057] Figure 5 Schematic diagram of the conductivity change curve at the upper and lower ends of the scaled glass liquid collector.

[0058] 1. Micro-injection pump, 2. Temperature-resistant and pressure-resistant intermediate container for storing the water phase, 3. Temperature-resistant and pressure-resistant intermediate container for storing the oil phase, 4. Flow controller, 5. Nested micro-injector, 6. Core holder, 7. Digital pressure controller, 8. Artificial core model, 9. Confining pressure device, 10. Syringe-type droplet ejector, 11. Hydrophilic ceramic plate, 12. Visual glass observation window, 13. 500x microscope, 14. High-speed camera, 15. Six-way valve, 16. Computer, 17. Adjustable distance bracket, 18. Capillary bundle model , 19. Measuring cylinder, 20. Conductivity meter, 21. Glass collecting tube with scale, 22. Conductivity probe, 23. Conductivity analysis system, 24. Output liquid collection device, 25. Inner tube, 26. Outer tube, 27. Inlet conduit, 28. Cap, 29. Fixed steel sleeve, 30. Sealing ring, 31. Telescopic controller, 32. Flexible hinge displacement groove, 33. Fluid chamber, 34. Telescopic plate, 35. One-way valve, 36. Neck hole, 37. Outlet conduit, 38. Microfluidic control piece, 39. Micropore, 40. Micro differential pressure gauge. DETAILED DESCRIPTION

[0059] The present invention will be described in detail below with reference to the accompanying drawings and embodiments, but is not limited thereto.

[0060] Example 1

[0061] A multifunctional integrated experimental device for preparing and simultaneously measuring emulsion properties, such as Figure 1 As shown, it includes a fluid injection system, an emulsion generation system, an emulsion testing system and a produced fluid collection system;

[0062] During the experiment, the water phase and oil phase were pumped into the emulsion generation system through the fluid injection system. After the emulsion was generated, it entered the emulsion testing system through the six-way valve 15. The phase state, viscosity and stability of the emulsion were simultaneously measured. Finally, the emulsion was collected and processed by the production fluid collection system.

[0063] The present invention realizes the generation of emulsion in the porous medium of the core under high-pressure experimental conditions and the simultaneous determination of its phase state, viscosity and stability, and can provide a multifunctional integrated experimental device for further studying the generation and evolution characteristics of emulsion in porous media.

[0064] Example 2

[0065] The multifunctional integrated experimental device for preparing and simultaneously measuring the properties of emulsions described in Example 1 is different in that:

[0066] The fluid injection system includes a micro-injection pump 1, a temperature-resistant and pressure-resistant intermediate container, and a flow controller 4 connected in sequence; the temperature-resistant and pressure-resistant intermediate container includes a temperature-resistant and pressure-resistant intermediate container 2 for storing a water phase and a temperature-resistant and pressure-resistant intermediate container 3 for storing an oil phase;

[0067] The micro-injection pump 1 is connected to the temperature-resistant and pressure-resistant intermediate container 2 for storing the water phase and the temperature-resistant and pressure-resistant intermediate container 3 for storing the oil phase. The flow regulator 4 is connected to the inlet of the nested micro-injector 5 of the emulsion generation system to provide fluid injection conditions for emulsion generation.

[0068] A micro-injection pump 1 pumps distilled water into a heat-resistant and pressure-resistant intermediate container 2 for storing the water phase and a heat-resistant and pressure-resistant intermediate container 3 for storing the oil phase. A flow controller 4 adjusts the mixing ratio of the water and oil phases to simulate the emulsification of heavy oil in reservoirs under different water-containing conditions. The injected water phase consists of an aqueous solution of emulsifiers and stabilizers dissolved in formation water, while the injected oil phase is dehydrated crude oil extracted from an actual reservoir. The emulsifier in the water phase is an anionic surfactant, petroleum sulfonate RSO3M, where the R group represents a linear aliphatic alkyl group with an average carbon number of 14 to 18. The emulsifier has a density of 1.08 g / ml, a solids content of 45%, an HLB value of 8 to 11, and a mass percentage of 0.1% to 1% in the water phase. The stabilizer in the water phase is aluminum oxide nanoparticles with an average diameter of 20 nm and a mass fraction of 0.1% to 0.2%.

[0069] The emulsion generation system includes a digital pressure controller 7, a nested micro-injector 5, a core holder 6, an artificial core model 8, and a confining pressure device 9; the outlet end of the nested micro-injector 5 is connected to the inlet end of the core holder 6 and the digital pressure controller 7, the artificial core model 8 is placed in the core holder 6, and the core holder 6 is connected to the confining pressure device 9;

[0070] Among them, the digital pressure controller 7 is used to collect the injection pressure during the emulsion generation and seepage process, the artificial core model 8 is used to simulate the generation of emulsion in porous media, and the confining pressure device 9 is used to control the pressure state in the artificial core model 8.

[0071] The artificial rock core model 8 is a cylinder with a length of 5 cm and a diameter of 2.5 cm.

[0072] like Figure 2 As shown, the nested microinjector 5 consists of an inner tube 25 and an outer tube 26 nested together. The inner tube 25 is embedded within the outer tube 26. The inner and outer tubes 25 and 26 are axially parallel and welded together. The inner tube 25 has a diameter of 2 mm, the outer tube 26 has a diameter of 5 mm, and the pressure-resistant tube wall thickness is 1 mm. The tail of the nested microinjector 5 is a conical manifold with a one-way flow valve installed at the conical manifold. During the experiment, the water phase was pumped in through the outer tube 26, and the oil phase was pumped in through the inner tube 25. The water and oil phases were pumped into the artificial core model 8 through the conical manifold using a coaxial fluid focusing method.

[0073] The emulsion testing system includes a phase determination device, a viscosity measurement device and a stability analysis device;

[0074] The phase determination device is used to measure the phase state of the emulsion; the viscosity measuring device is used to measure the viscosity of the emulsion; and the stability analysis device is used to measure the stability of the emulsion.

[0075] The phase determination device includes a syringe-type droplet ejector 10, an 80 mm x 80 mm square hydrophilic ceramic plate 11, a visual glass observation window 12, and an adjustable distance bracket 17. The syringe-type droplet ejector 10 is connected to a six-way valve 15, and the hydrophilic ceramic plate 11 is perpendicular to the outlet end of the syringe-type droplet ejector 10.

[0076] The syringe-type droplet ejector 10 sprays the emulsion in the form of droplets onto the hydrophilic ceramic plate 11. The hydrophilic ceramic plate 11 controls the distribution of the different phases of the emulsion sprayed onto the hydrophilic ceramic plate 11 through its surface hydrophilicity. Specifically, the hydrophilic ceramic plate 11 can aggregate the water-in-oil emulsion into droplets and spread the oil-in-water emulsion into a thin film.

[0077] The visual glass observation window 12 is used to microscopically observe the occurrence state of the emulsion on the surface of the hydrophilic ceramic plate 11;

[0078] The adjustable distance bracket 17 controls the distance between the hydrophilic ceramic plate 11 and the outlet end of the syringe-type droplet ejector 10 by rotating the spiral;

[0079] The phase determination device also includes a 500x microscope 13, a high-speed camera 14 and a computer 16; the microscope is installed directly above the hydrophilic ceramic plate 11 and is connected to the high-speed camera 14 and the computer 16 for determining the phase of the generated emulsion.

[0080] like Figure 3As shown, the syringe droplet ejector 10 includes an inlet conduit 27, a cap 28, a fixed steel sleeve 29, a sealing ring 30, a telescopic controller 31, a flexible hinge displacement groove 32, a fluid chamber 33, a telescopic plate 34, a one-way valve 35, a necking hole 36, an outlet conduit 37 and a microfluidic control sheet 38;

[0081] A cap 28 is provided on the left side of the fluid chamber 33. Fixed steel sleeves 29 are provided on the upper and lower sides of the fluid chamber 33. The space formed by the cap 28 and the fixed steel sleeve 29 is the fluid chamber 33. A flexible hinge displacement groove 32 and a sealing ring 30 are provided in sequence below the fixed steel sleeve 29 on the upper side of the fluid chamber 33. A flexible hinge displacement groove 32 and a sealing ring 30 are provided in sequence above the fixed steel sleeve 29 on the lower side of the fluid chamber 33. A telescopic plate 34 is provided longitudinally within the fluid chamber 33, dividing the fluid chamber 33 into the fluid chamber 33 at the front end of the telescopic plate 34 and the fluid chamber 33 at the rear end of the telescopic plate 34. A one-way valve 35 is provided on the telescopic plate 34. A necking hole 36, an outlet conduit 37 and a microfluidic control plate 38 are provided in sequence on the right side of the fluid chamber 33. A micropore 39 is provided on the microfluidic control plate 38.

[0082] During the experiment, the emulsion enters the fluid chamber 33 at the front end of the telescopic plate 34 through the inlet conduit 27 and then passes through the one-way valve 35 to enter the fluid chamber 33 at the rear end of the telescopic plate 34. The telescopic controller 31 controls the telescopic plate 34 to rapidly move along the flexible hinge displacement groove 32 toward the outlet conduit 37, thereby rapidly pressurizing the fluid chamber 33 at the rear end of the telescopic plate 34. This forces the emulsion through the constriction hole 36 and into the outlet conduit 37, ultimately ejecting it through the micropores 39 on the microfluidic control plate 38 at the end of the outlet conduit 37. After each ejection cycle, the telescopic controller 31 controls the telescopic plate 34 to slowly move along the flexible hinge displacement groove 32 toward the inlet conduit 27, forcing the emulsion in the fluid chamber 33 at the front end of the telescopic plate 34 to reenter the fluid chamber 33 at the rear end of the telescopic plate 34 through the one-way valve 35, repeating the ejection process. After the experiment, the cap 28 can be removed and solvent can be injected to clean the ejector cavity.

[0083] The cover cap 28 and the fixed steel sleeve 29 are made of 303 stainless steel.

[0084] The viscosity measuring device includes a capillary bundle model 18, a measuring cylinder 19, and a micro differential pressure gauge 40; wherein the inlet end of the capillary bundle model 18 is connected to the six-way valve 15, the outlet end of the capillary bundle model 18 is connected to the measuring cylinder 19, and the micro differential pressure gauge 40 is connected to the inlet and outlet ends of the capillary bundle model 18 respectively;

[0085] During the experiment, the volume of the emulsion flowing through the capillary bundle model 18 per unit time is collected by a measuring cylinder 19, and the pressure difference at both ends of the capillary bundle model 18 is measured by a micro differential pressure meter 40, based on which the viscosity of the emulsion is calculated.

[0086] The stability analysis device includes a conductivity meter 20, a graduated glass liquid collecting tube 21, a conductivity probe 22, and a conductivity analysis system 23;

[0087] A graduated glass collection tube 21 is connected to the six-way valve 15. A conductivity probe 22 of the conductivity meter 20 is placed one-third of the way from the bottom of the graduated glass collection tube 21 and is connected to a conductivity analysis system 23. The electrode mounted on the conductivity probe 22 is platinum-plated to increase fluid conductivity. The conductivity analysis system 23 collects the emulsion conductivity signal in real time and analyzes conductivity changes.

[0088] During the experiment, electrodes installed at different positions on the conductivity probe 22 accurately measure the liquid conductivity signal at that position and transmit it to the conductivity analysis system 23 through a wire. At the same time, a conductivity value change curve at different times and positions is plotted. If the conductivity values ​​at different times and positions are constant, it indicates that the emulsion is relatively stable. If the conductivity value at the upper end of the graduated glass collecting tube 21 decreases and the conductivity value at the lower end increases within a certain period of time, it indicates that the emulsion has broken and stratified, and its stability is relatively poor.

[0089] The output liquid collection system is a output liquid collection device 24 , the inlet end of which is connected to a six-way valve 15 to collect the remaining emulsion during the experiment.

[0090] Example 3

[0091] The working method of the multifunctional integrated experimental device for preparing emulsions and simultaneously determining their properties as described in Example 2 includes:

[0092] The water phase and oil phase are pumped into the emulsion generation system through the fluid injection system; after the emulsion is generated in the emulsion generation system, it enters the emulsion testing system through the six-way valve 15, and the phase state, viscosity and stability of the emulsion are simultaneously measured. Finally, it is collected and processed by the production fluid collection system.

[0093] The working method of the multifunctional integrated experimental device for preparing emulsions and simultaneously measuring their properties comprises the following specific steps:

[0094] (1) The aqueous solution formed by dissolving the emulsifier and stabilizer in the formation water is stored in a temperature-resistant and pressure-resistant intermediate container as the experimental water phase, and the crude oil produced from the actual oil reservoir is dehydrated and stored in a temperature-resistant and pressure-resistant intermediate container as the experimental oil phase; the injection rate of the water phase and the oil phase is regulated by the micro-injection pump 1 and the flow controller 4, and the back pressure in the experiment is set by the confining pressure device 9;

[0095] (2) The oil phase and the water phase are injected into the artificial core model 8 through the inner tube 25 and the outer tube 26 of the nested micro-injector 5 respectively to generate an emulsion, which flows into the six-way valve 15 through the outlet end of the artificial core model 8 and enters the emulsion testing system;

[0096] (3) In the phase determination experiment, the emulsion enters the syringe droplet ejector 10 through the six-way valve 15, and the adjustable distance bracket 17 between the square hydrophilic ceramic plate 11 and the syringe droplet ejector 10 is adjusted so that the emulsion is deposited on the square hydrophilic ceramic plate 11 after passing through the microfluidic control plate 38 including the 3×3 micropores 39. The state of the emulsion in the visual glass observation window 12 is observed by a microscope and a high-speed camera 14. If the emulsion forms liquid droplets on the square hydrophilic ceramic plate 11, it is an oil-in-water emulsion. If the emulsion forms a thin emulsion film on the square hydrophilic ceramic plate 11, it is an oil-in-water emulsion. During the experiment, the emulsion state is stored by a computer 16; Figure 4 The figure shows a micrograph of the experimentally measured emulsion spreading as a thin emulsion film. Based on the above analysis, it can be determined that the emulsion phase is an oil-in-water type.

[0097] In the viscosity measurement experiment, the emulsion enters the inlet of the capillary bundle model 18 through the six-way valve 15, flows through the capillary bundle model 18, and enters the measuring cylinder 19 through the outlet for collection. The volume of the emulsion flowing through the capillary bundle model 18 per unit time is measured. At the same time, a micro differential pressure meter 40 is used to measure the pressure difference between the two ends of the capillary bundle model 18 during the flow of the emulsion. Based on this, the viscosity of the emulsion is calculated.

[0098] The calculation formula of the viscosity of the emulsion is shown in formula (I):

[0099]

[0100] In formula (I), η represents the viscosity of the emulsion, Q represents the volume of the emulsion flowing through the capillary bundle model 18 per unit time, which is 0.001 cm 3 ; ΔP represents the pressure difference across the capillary bundle model 18, which is 1.2 Pa; n represents the number of parallel capillaries arranged in the capillary bundle model 18, which is 5; r represents the radius of each capillary, which is 0.1 cm; L represents the length of each capillary, which is 5 cm; the viscosity of the emulsion is calculated to be 47.1 mPa.s;

[0101] In the stability analysis experiment, the emulsion enters the graduated glass collecting tube 21 through the six-way valve 15. The electrodes installed at different positions on the conductivity probe 22 accurately measure the liquid conductivity signal at that position and transmit it to the conductivity analysis system 23 through a wire. At the same time, a conductivity value change curve at different times and different positions is plotted. If the conductivity values ​​at different times and different positions are constant, it indicates that the emulsion is relatively stable. If the conductivity value at the upper end of the graduated glass collecting tube 21 decreases and the conductivity value at the lower end increases within a certain period of time, it indicates that the emulsion has broken and separated, and the stability is poor. Figure 5 As shown in the figure, it can be seen that after a certain period of time, the conductivity value at the upper end of the collecting pipe decreases and the conductivity value at the lower end increases, indicating that the emulsion breaks and stratifies, so the stability is poor;

[0102] The excess emulsion generated during the experiment enters the output fluid collection device 24 through the six-way valve 15 for collection and treatment.

[0103] The present invention realizes the generation of emulsion in the porous medium of the core under high-pressure experimental conditions and the simultaneous determination of its phase state, viscosity and stability, and can provide a multifunctional integrated experimental device for further studying the generation and evolution characteristics of emulsion in porous media.

Claims

1. A multifunctional integrated experimental device for preparing emulsions and simultaneously measuring their properties, characterized in that: Includes fluid injection system, emulsion generation system, emulsion testing system and produced fluid collection system; During the experiment, the water phase and oil phase were pumped into the emulsion generation system through the fluid injection system. After the emulsion was generated, it entered the emulsion testing system, where the phase state, viscosity, and stability of the emulsion were simultaneously measured. Finally, the produced fluid collection system collected and processed it. The emulsion testing system includes a phase determination device, a viscosity measurement device and a stability analysis device; The phase determination device is used to measure the phase state of the emulsion; the viscosity measuring device is used to measure the viscosity of the emulsion; the stability analysis device is used to measure the stability of the emulsion; The phase determination device includes a syringe-type droplet ejector, a hydrophilic ceramic plate, a visual glass observation window, and an adjustable distance bracket; the hydrophilic ceramic plate is perpendicular to the outlet end of the syringe-type droplet ejector; The syringe-type droplet ejector sprays the emulsion in the form of droplets onto the hydrophilic ceramic plate; the hydrophilic ceramic plate controls the occurrence form of the different phases of the emulsion sprayed onto the hydrophilic ceramic plate through its surface hydrophilic properties; The visual glass observation window is used to microscopically observe the occurrence morphology of the emulsion on the surface of the hydrophilic ceramic plate; The adjustable distance bracket controls the distance between the hydrophilic ceramic plate and the outlet end of the syringe-type droplet ejector by rotating the screw; The syringe droplet ejector comprises an inlet conduit, a cap, a fixed steel sleeve, a sealing ring, a telescopic controller, a flexible hinge displacement groove, a fluid chamber, a telescopic plate, a one-way valve, a necking hole, an outlet conduit and a microfluidic control sheet; A cap is provided on the left side of the fluid chamber, and fixed steel sleeves are provided on the upper and lower sides of the fluid chamber. The space formed by the cap and the fixed steel sleeve is the fluid chamber; a flexible hinge displacement groove and a sealing ring are provided in sequence below the fixed steel sleeve on the upper side of the fluid chamber; a flexible hinge displacement groove and a sealing ring are provided in sequence above the fixed steel sleeve on the lower side of the fluid chamber; a telescopic plate is provided longitudinally within the fluid chamber, dividing the fluid chamber into a fluid chamber at the front end of the telescopic plate and a fluid chamber at the rear end of the telescopic plate, and a one-way valve is provided on the telescopic plate; a necking hole, an outlet conduit and a microfluidic control plate are provided in sequence on the right side of the fluid chamber; and micropores are provided on the microfluidic control plate. During the experiment, the emulsion entered the fluid chamber at the front end of the telescopic plate through the inlet tube and then passed through a one-way valve into the fluid chamber at the rear end of the plate. The telescopic controller caused the plate to rapidly move along the flexible hinge displacement groove toward the outlet tube, thereby rapidly pressurizing the fluid chamber at the rear end of the plate. This pushed the emulsion through the constriction hole into the outlet tube and was ultimately ejected from the micropores on the microfluidic control plate at the end of the outlet tube. Each time a spray is completed, the telescopic controller controls the telescopic plate to move slowly along the flexible hinge displacement groove toward the inlet conduit, causing the emulsion in the fluid chamber at the front end of the telescopic plate to enter the fluid chamber at the rear end of the telescopic plate through the one-way valve again, repeating the above spray process.

2. The multifunctional integrated experimental device for preparing and simultaneously measuring emulsion properties according to claim 1, characterized in that: The fluid injection system includes a micro-injection pump, a temperature-resistant and pressure-resistant intermediate container, and a flow controller connected in sequence; the temperature-resistant and pressure-resistant intermediate container includes a temperature-resistant and pressure-resistant intermediate container for storing a water phase and a temperature-resistant and pressure-resistant intermediate container for storing an oil phase; A micro-injection pump pumps distilled water into and drives the pistons in the temperature-resistant and pressure-resistant intermediate container for storing the water phase and the temperature-resistant and pressure-resistant intermediate container for storing the oil phase; a flow controller adjusts the mixing ratio of the water phase and the oil phase to simulate the emulsification of heavy oil in the reservoir under different water content conditions.

3. The multifunctional integrated experimental device for preparing and simultaneously measuring the properties of emulsions according to claim 2, characterized in that: The emulsion generation system includes a digital pressure controller, a nested micro-injector, a core holder, an artificial core model, and a confining pressure device; the outlet end of the nested micro-injector is connected to the inlet end of the core holder and the digital pressure controller, the artificial core model is placed in the core holder, and the core holder is connected to the confining pressure device; Among them, the digital pressure controller is used to collect the injection pressure during the emulsion formation and seepage process, the artificial core model is used to simulate the formation of emulsion in porous media, and the confining pressure device is used to control the pressure state inside the artificial core model.

4. The multifunctional integrated experimental device for preparing and simultaneously measuring emulsion properties according to claim 3, characterized in that: The artificial core model is a cylinder.

5. The multifunctional integrated experimental device for preparing and simultaneously measuring the properties of emulsion according to claim 3, characterized in that: The nested micro-injector is composed of an inner tube and an outer tube nested together, the inner tube is embedded in the outer tube, and the inner and outer tubes are axially parallel and fixed; the tail of the nested micro-injector is a conical collection port. During the experiment, the water phase is pumped in through the outer tube and the oil phase is pumped in through the inner tube. The water phase and the oil phase are pumped into the artificial core model through the conical collection port in a coaxial fluid focusing manner.

6. The multifunctional integrated experimental device for preparing and simultaneously measuring the properties of emulsions according to claim 5, characterized in that: The phase determination device also includes a microscope, a high-speed camera and a computer; The microscope is installed just above the hydrophilic ceramic plate and is connected to a high-speed camera and a computer to determine the phase state of the generated emulsion.

7. The multifunctional integrated experimental device for preparing and simultaneously measuring emulsion properties according to claim 1, characterized in that: The cover cap and fixed steel sleeve are made of 303 stainless steel.

8. The multifunctional integrated experimental device for preparing and simultaneously measuring emulsion properties according to claim 6, characterized in that: The viscosity measuring device includes a capillary bundle model, a graduated cylinder, and a micro differential pressure gauge; wherein the inlet end of the capillary bundle model is connected to the emulsion input pipeline, the outlet end of the capillary bundle model is connected to the graduated cylinder, and the micro differential pressure gauge is connected to the inlet end and the outlet end of the capillary bundle model respectively; During the experiment, the volume of the emulsion flowing through the capillary bundle model per unit time was collected using a graduated cylinder, and the pressure difference at both ends of the capillary bundle model was measured using a micro-differential pressure meter. Based on this, the viscosity of the emulsion was calculated.

9. The multifunctional integrated experimental device for preparing and simultaneously measuring the properties of emulsions according to claim 8, characterized in that: The stability analysis device includes a conductivity meter, a glass liquid collecting tube with a scale, a conductivity probe, and a conductivity analysis system; The conductivity probe of the conductivity meter is placed at the bottom of a graduated glass collecting tube and connected to a conductivity analysis system. The conductivity analysis system collects the conductivity signal of the emulsion in real time and analyzes the conductivity changes. During the experiment, electrodes installed at different positions on the conductivity probe accurately measure the liquid conductivity signal at that position and transmit it to the conductivity analysis system through wires. At the same time, a conductivity value change curve at different times and positions is plotted. If the conductivity values ​​at different times and positions are constant, it indicates that the emulsion is relatively stable. If the conductivity value at the upper end of the graduated glass collecting tube decreases and the conductivity value at the lower end increases within a certain period of time, it indicates that the emulsion has broken and stratified, and its stability is poor.

10. The multifunctional integrated experimental device for preparing and simultaneously measuring emulsion properties according to claim 9, characterized in that: The produced fluid collection system is a produced fluid collection device that collects the remaining emulsion during the experiment.

11. The operating method of the multifunctional integrated experimental device for preparing and simultaneously measuring the properties of emulsions according to claim 10, characterized in that: The specific steps include: (1) The aqueous solution formed by dissolving the emulsifier and stabilizer in the formation water is stored as the experimental water phase in a temperature-resistant and pressure-resistant intermediate container, and the crude oil produced from the actual oil reservoir is dehydrated and stored as the experimental oil phase in a temperature-resistant and pressure-resistant intermediate container; the injection rate of the water phase and the oil phase is regulated by a micro-injection pump and a flow controller, and the confining pressure in the experiment is set by a confining pressure device; (2) injecting the oil phase and the water phase into the artificial core model through the inner tube and outer tube of the nested microinjector respectively to generate an emulsion, which flows into the six-way valve through the outlet of the artificial core model and enters the emulsion testing system; (3) In the phase determination experiment, the emulsion enters the syringe droplet ejector through the six-way valve. The adjustable distance bracket between the hydrophilic ceramic plate and the syringe droplet ejector is adjusted so that the emulsion is deposited on the hydrophilic ceramic plate after passing through the microfluidic control plate. The state of the emulsion in the visual glass observation window is observed by a microscope and a high-speed camera. If the emulsion forms liquid droplets on the hydrophilic ceramic plate, it is an oil-in-water emulsion. If the emulsion forms a thin emulsion film on the hydrophilic ceramic plate, it is an oil-in-water emulsion. The emulsion state is stored by a computer. In the viscosity measurement experiment, the emulsion enters the inlet of the capillary bundle model through a six-way valve, flows through the capillary bundle model, and enters the graduated cylinder at the outlet for collection. The volume of the emulsion flowing through the capillary bundle model per unit time is measured. At the same time, a micro-differential pressure gauge is used to measure the pressure difference between the two ends of the capillary bundle model during the emulsion flow. Based on this, the viscosity of the emulsion is calculated. In the stability analysis experiment, the emulsion enters a graduated glass manifold through a six-way valve. Electrodes installed at different locations on the conductivity probe accurately measure the liquid conductivity signal at that location and transmit it to the conductivity analysis system via wires. A curve of conductivity values ​​at different times and locations is simultaneously plotted. If the conductivity values ​​remain constant at different times and locations, the emulsion is considered stable. If the conductivity value at the upper end of the graduated glass manifold decreases while the conductivity value at the lower end increases over a certain period of time, the emulsion is experiencing demulsification and separation, indicating poor stability. The excess emulsion generated during the experiment enters the produced fluid collection device through a six-way valve for collection and treatment.

12. The working method of the multifunctional integrated experimental device for emulsion preparation and simultaneous property determination according to claim 11, characterized in that: The calculation formula of the viscosity of the emulsion is shown in formula (I): In formula (I), η represents the viscosity of the emulsion, Q represents the volume of the emulsion flowing through the capillary bundle model per unit time, ΔP represents the pressure difference across the capillary bundle model, n represents the number of parallel capillaries arranged in the capillary bundle model, r represents the radius of each capillary, and L represents the length of each capillary.

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