Device and experimental method for measuring emulsion strength stability of emulsion

By combining specially designed test tubes and centrifuges with light intensity and grayscale data acquisition, the problem of emulsion stability testing after oil well acidizing was solved, enabling rapid separation and stability assessment of the emulsion, and improving the efficiency of acidizing operations and resource utilization.

CN120870064AActive Publication Date: 2025-10-31SANYA MARINE OIL & GAS RESEARCH INSTITUTE NORTHEAST PETROLEUM UNIVERSITY +1
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Patent Information

Application Number
CN202511367178.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-24
Publication Date
2025-10-31
Estimated Expiration
2045-09-24

AI Technical Summary

Technical Problem

The emulsion produced after oil well acidizing is highly stable and difficult to demulsify and separate using conventional methods, which affects the treatment efficiency and cost of acidizing flowback fluid and results in serious waste of crude oil resources.

Method used

Using specially designed test tubes and a centrifuge, the stability of emulsions is detected by acquiring light intensity and grayscale data. Data is collected using light intensity and grayscale sensors, and transmitted via a magnetic transmission structure. Computer analysis of image change patterns enables rapid stratification and stability assessment of the emulsion.

Benefits of technology

It enables rapid separation and stability testing of emulsions, improves the efficiency of acidizing operations, promotes the sustainable development and environmental protection of oilfields, and provides theoretical support for the research on the reuse of acidizing backflow fluid.

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Abstract

The invention discloses a device for measuring emulsion intensity stability of emulsion, and belongs to the field of oilfield acidification reverse discharge liquid detection.The device comprises a centrifugal machine and a computer connected with the centrifugal machine, a centrifugal test tube rack is installed in the centrifugal machine, and a plurality of special test tubes are arranged on the centrifugal test tube rack; the special test tube is connected with the centrifugal test tube rack through a vertical rotating structure, and is provided with a magnetic suction transmission structure for magnetic suction fixation and data transmission; the special test tube comprises a test tube body, and a light source for emitting light, a light intensity sensor for receiving intensity data of light penetrating through the emulsion and a gray scale sensor for receiving gray scale data of the emulsion irradiated by the light are arranged in the test tube body. The special test tube with a light intensity and gray scale data acquisition function is matched with the centrifugal machine, so that the emulsion intensity stability detection of the emulsion is realized simply, quickly and efficiently, the detection technology of the acidified reverse discharge liquid is perfected, and a theoretical support is provided for the continuous development of subsequent acidified reverse discharge liquid reutilization research.
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Description

Technical Field

[0001] This invention relates to the field of oilfield acidizing backflow fluid detection technology, and in particular to an apparatus and experimental method for determining the emulsion strength stability of emulsions. Background Technology

[0002] During long-term water injection development of oil reservoirs, scaling in the near-wellbore formation reduces the injection capacity of injection wells, directly leading to a significant decrease in injection efficiency. This scaling phenomenon not only limits water injection efficiency but also increases operating costs, posing a serious challenge to the continuous and efficient development of oil fields. To address this issue, acidizing technology has emerged and quickly become an important component of oil field production enhancement measures.

[0003] For oil wells, acidizing can significantly enhance the permeability of the near-wellbore zone, allowing crude oil to flow more smoothly into the wellbore and thus increasing the well's fluid production. For injection wells, acidizing can remove blockages caused by scaling, ensuring that injection media such as water or polymers can smoothly enter the formation and maintain or improve water injection efficiency.

[0004] However, well acidizing also brings a series of new problems, the most prominent of which is the emulsification phenomenon caused by the mixing of crude oil and flowback fluid. This emulsion is not only highly stable and difficult to demulsify and separate using conventional methods, but it also has a high crude oil content, severely impacting the treatment efficiency and cost of acidizing flowback fluid. Even more seriously, if the crude oil in the emulsion cannot be effectively recovered, it will result in a huge waste of resources and environmental pollution.

[0005] Currently, there is a lack of in-depth research on the emulsification mechanism of crude oil in the flowback fluid after acidizing. Unlike the emulsification mechanism of conventional crude oil, the emulsification mechanism of acidized crude oil is more complex, making it difficult for conventional treatment methods to meet requirements. The emulsification problem of crude oil in acidizing flowback fluid severely affects its treatment. This research not only helps improve the effectiveness and efficiency of acidizing operations but also promotes the sustainable development of oilfields and environmental protection. Furthermore, it is of great significance for advancing technological progress in oilfield chemistry and oil production engineering. Summary of the Invention

[0006] The purpose of this invention is to provide an apparatus and experimental method for determining the emulsion strength stability of emulsions. By using a specially designed test tube with light intensity and grayscale data acquisition functions in conjunction with a centrifuge, data acquisition, transmission, processing and analysis can be realized, achieving simple, fast and efficient detection of emulsion strength stability, improving the technology for detecting acidified backflow liquid, and providing theoretical support for the continued development of research on the reuse of acidified backflow liquid.

[0007] To achieve the above objectives, the present invention provides an apparatus for determining the emulsion strength stability of an emulsion, comprising a centrifuge and a computer connected to the centrifuge. The centrifuge contains a centrifuge tube rack, on which several specially designed test tubes are arranged. The specially designed test tubes are connected to the centrifuge tube rack via a vertical rotation structure. Each specially designed test tube is equipped with a magnetic attraction transmission structure for magnetic fixation and data transmission. Each specially designed test tube includes a test tube body, inside which are arranged a light source for emitting light, a light intensity sensor for receiving light intensity data transmitted through the emulsion, and a grayscale sensor for receiving grayscale data of the emulsion after irradiation by light.

[0008] Preferably, the vertical rotation structure includes several fixing components for fixing special test tubes, and the two ends of the fixing components are rotatably connected to the centrifuge test tube rack.

[0009] Preferably, the centrifuge tube rack is provided with an opening for accommodating specially designed test tubes after vertical rotation.

[0010] Preferably, the magnetic transmission structure includes a magnetic protrusion on a special test tube, a magnetic groove on a fixing member that matches the magnetic protrusion, and metal contacts for data transmission on the magnetic protrusion and the magnetic groove.

[0011] Preferably, the magnetic transmission structure achieves power supply and data transmission through a slip ring structure.

[0012] Preferably, the light source is located at the center inside the test tube body.

[0013] Preferably, the light intensity sensor and the grayscale sensor are arranged evenly in a circular pattern on the inner wall of the test tube.

[0014] This invention provides an experimental method for determining the emulsion strength stability of an emulsion, comprising the following steps: Step 1: Take the emulsion in its natural state and pour an equal amount into a special test tube; Step two: Insert the special test tubes into the centrifuge tube rack of the centrifuge and secure them magnetically; Step 3: Turn on the computer, analyze and record the initial images, and adjust the light intensity of the light source in the test tube using computer control. Step 4: Turn on the centrifuge and perform an initial rotation test; Step 5: Once everything is ready, turn the centrifuge on full speed, set the rotation speed, and conduct a test for the specified time. Step 6: The light intensity sensor and grayscale sensor collect light intensity data and grayscale data respectively and transmit them to the computer in real time. The computer's decision-making and image display are viewed, the final result and time of emulsion stratification are recorded, and the change pattern of the image is analyzed. Step 7: Once the computer display stops changing or the predetermined time has elapsed, turn off the centrifuge.

[0015] Therefore, the present invention, employing the above-mentioned apparatus and experimental method for determining the emulsion strength stability of an emulsion, has the following beneficial effects: 1. This invention solves the problem of the lack of a sound method for detecting the emulsion strength and stability. The process is simple and can process the stability of the emulsion at various times, as well as the emulsion separation rate and separation time, to obtain various properties of the emulsion itself related to stability. It can monitor and make decisions at any time, and digitize the entire process of emulsion changes, which helps to improve the effect and efficiency of acidizing operations and promote the sustainable development of oil fields and environmental protection.

[0016] 2. The specially designed test tube in this invention collects light intensity and grayscale data during centrifugation. Combined with the raised points and grooves of the magnetic data transmission, it improves the convenience of detection and avoids improper operation and differences by the experimenter, thus realizing a simple, fast and efficient detection of the emulsion strength and stability.

[0017] 3. This invention is used to detect and analyze the emulsion strength stability, obtain various analytical images, analyze the characteristic changes during the emulsion layering process, and analyze the emulsion strength stability to facilitate subsequent research and secondary utilization of the backflow liquid.

[0018] 4. Using the experimental methods and equipment provided by this invention, the stability trends of emulsions of various types and compositions are analyzed, their own characteristics are analyzed, and the effects are evaluated, providing theoretical support for the continued development of research on the reuse of acidified backflow liquid.

[0019] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of the device for determining the emulsion strength stability of an emulsion according to an embodiment of the present invention; Figure 2 This is a front view of a centrifuge tube rack according to an embodiment of the present invention; Figure 3 This is a top view of a centrifuge tube rack according to an embodiment of the present invention; Figure 4 This is a schematic diagram of the vertical rotation of a specially designed test tube during centrifugation, according to an embodiment of the present invention. Figure 5 This is a schematic diagram of the internal structure of a specially designed test tube according to an embodiment of the present invention; Figure 6 This is a top view of a specially designed test tube according to an embodiment of the present invention.

[0021] Figure Labels 1. Special test tube; 2. Test tube body; 3. Light source; 4. Magnetic protrusion; 5. Centrifuge tube rack; 6. Magnetic groove; 7. Slip ring structure; 8. Opening; 9. Fixing component; 10. Centrifuge; 11. Light intensity sensor; 12. Gray scale sensor. Detailed Implementation

[0022] To make the objectives, technical solutions, and advantages disclosed in the embodiments of the present invention clearer, the embodiments of the present invention will be further described in detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the embodiments of the present invention and are not intended to limit the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments in this application without creative effort are within the scope of protection of this application. Examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout.

[0023] It should be noted that the terms “comprising” and “having”, and any variations thereof, are intended to cover non-exclusive inclusion, such that a process, method, system, product, or server that includes a series of steps or units is not necessarily limited to those steps or units that are explicitly listed, but may include other steps or units that are not explicitly listed or that are inherent to such processes, methods, products, or devices.

[0024] Similar labels and letters in the following figures indicate similar items; therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0025] In the description of this invention, it should be noted that the terms "upper," "lower," "inner," "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship in which the product of this invention is usually placed when in use. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limiting this invention.

[0026] In the description of this invention, it should also be noted that, unless otherwise explicitly specified and limited, the terms "set," "install," and "connect" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0027] Example like Figure 1 , Figure 2 As shown, the apparatus for determining the emulsion strength stability of an emulsion according to the present invention includes a centrifuge 10 and a computer connected to the centrifuge 10. The centrifuge 10 is a TDZ5-WS / TDZ5WS type centrifuge. A centrifuge tube rack 5 is installed inside the centrifuge 10, and a number of specially made test tubes 1 are arranged on the centrifuge tube rack 5.

[0028] like Figure 5 , Figure 6 As shown, the specially designed test tube 1 includes a test tube body 2. Inside the test tube body 2 are a light source 3 for emitting light, a light intensity sensor 11 for receiving light intensity data transmitted through the emulsion, and a grayscale sensor 12 for receiving grayscale data of the emulsion after illumination. The test tube body 2 is a specially designed functional test tube made of stainless steel to avoid reaction with residual acid in the acidified reflux solution or other chemical agents. The light source 3 is located at the center inside the test tube body 2 and uses a laser light source, allowing for adjustable light intensity. The light intensity sensor 11 and grayscale sensor 12 are evenly arranged circumferentially on the inner wall of the test tube, with the light intensity sensor 11 and grayscale sensor 12 spaced apart. There is a grayscale sensor 12 between two adjacent light intensity sensors 11, and a light intensity sensor 11 between two adjacent grayscale sensors 12. By changing different light intensities, the visual effect is optimized, resulting in clearer and more accurate imaging.

[0029] like Figure 2 , Figure 3 , Figure 4 As shown, the special test tube 1 is connected to the centrifuge tube rack 5 via a vertical rotation structure. The vertical rotation structure includes several fixing parts 9 for fixing the special test tube 1, and both ends of the fixing parts 9 are rotatably connected to the centrifuge tube rack 5. The centrifuge tube rack 5 is provided with an opening 8 for accommodating the special test tube 1 after vertical rotation. The centrifuge tube rack 5 is fixed to the turntable of the centrifuge 10, and the fixing parts 9 on the centrifuge tube rack 5 can rotate vertically in the centrifuge turntable 10. When the rotation speed is high, it can be in an almost horizontal state, and the special centrifuge tube can be fixed on the fixing parts 9 and rotate accordingly.

[0030] The specially designed test tube 1 is equipped with a magnetic attraction transmission structure for magnetic fixation and data transmission. The magnetic attraction transmission structure includes a magnetic protrusion 4 on the test tube 1, and a magnetic groove 6 on the fixing component 9 that matches the magnetic protrusion 4. Metal contacts for data transmission are provided on the magnetic protrusion 4 and the magnetic groove 6. Power supply and data transmission are achieved through an existing slip ring structure 7.

[0031] The present invention provides an experimental method for determining the emulsion strength stability of an emulsion, comprising the following steps: Step 1: Take the emulsion in its natural state and pour an equal amount into a special test tube 1.

[0032] Step 2: Insert the special test tube 1 into the centrifuge tube rack 5 of the centrifuge 10, and adjust the test tube so that the magnetic protrusion 4 and the magnetic indentation attract and fix it.

[0033] Step 3: Turn on the computer, analyze and record the initial images, and adjust the light intensity of light source 3 in the test tube using computer control to achieve the best results.

[0034] Step 4: Turn on centrifuge 10 and perform an initial rotation test to avoid jamming or shaking.

[0035] Step 5: Once everything is ready without any unexpected issues, fully start the centrifuge (10), set the speed, and conduct a test for the specified time.

[0036] Step six: The light intensity sensor 11 and the grayscale sensor 12 collect light intensity data and grayscale data respectively and transmit them to the computer in real time. The computer makes decisions and displays images, records the final result and time of emulsion stratification, and analyzes the change pattern of the images.

[0037] The light intensity sensor 11 receives light transmitted through the emulsion, and the grayscale sensor 12 receives grayscale data transmitted through the emulsion. This data is transmitted to the centrifuge 10 via the magnetic protrusion 4, magnetic groove 6, and slip ring structure 7. The centrifuge 10 then transmits the data to the computer via a transmission line. The computer quantizes the collected data, derives the corresponding quantization stability value, and processes it using the quantization relationship between grayscale and stability to determine the corresponding quantization stability value and the position of each phase layer after centrifugation and stratification. The computer generates two images for comparison using both light intensity and grayscale data acquisition methods, avoiding errors caused by internal impurities, lighting factors, and other factors.

[0038] Step 7: Once the computer display no longer changes or the predetermined time has elapsed, the centrifuge 10 can be turned off.

[0039] This invention enables the detection and analysis of emulsion strength and stability, including but not limited to the determination of emulsification characteristics of acidified backflow solutions. The method is consistent for different emulsions or acidified backflow solutions; the above steps are repeated by changing the test tubes.

[0040] The method for quantifying emulsion stability employs a grayscale quantification method that promotes emulsification using ultrasound. The received light intensity is converted into a grayscale image, which is then processed according to the corresponding method studied.

[0041] The quantification method is briefly introduced below: The oil-water emulsion characteristics were quantitatively analyzed based on the captured emulsion images. All images were organized and batch-processed using image processing software Photoshop. The grayscale changes of the image near the oil-water interface over time were measured, and the concentration changes of the oil phase in the emulsion were calculated to analyze the emulsification rate.

[0042] Observations of oil-water emulsification at different times under ultrasonic treatment show that the oil and water phases gradually form an emulsion under ultrasonic treatment. The oil phase exists in the aqueous phase in the form of extremely small droplets. The emulsification rate to be measured can be characterized by the amount of crude oil emulsified per unit time. The longer the emulsification time, the more oil droplets are dispersed in the aqueous phase, and the darker the image color. This indicates that the method of measuring the emulsification rate by ultrasonic emulsification is feasible. At the same time, the observed images were uniformly converted to grayscale images, and the emulsification effect was characterized by analyzing the grayscale differences.

[0043] Based on the relationship between the velocity of the emulsion formed by ultrasonic vibration and the grayscale of the cuvette image, the actual image is converted into a grayscale image, and the grayscale change pattern of the cuvette at different locations and times is read using image recognition software and Python software.

[0044] After digitizing the image using the above method, grayscale curves were plotted at different times and locations. Simultaneously, the relationship between crude oil concentration and grayscale value after ultrasonic emulsification was obtained by using spectrophotometric absorbance standard curves for different oil contents. Figure 2 As shown.

[0045] To make the results more convincing, the centrifugation principle of centrifuge 10 is used as a basis for proof.

[0046] When an object moves in a circle around a central axis, a force pointing outwards from the circle is generated; this force is called centrifugal force. In centrifuge 10, a specially designed test tube 1 containing a sample is placed on a high-speed rotating turntable. As the rotation speed increases, the components in the sample are subjected to different degrees of centrifugal force due to differences in mass, density, or shape.

[0047] Centrifuge 10 utilizes centrifugal force generated by high-speed rotation to separate different components in the emulsion according to differences in density, size, or particle shape. Specifically, centrifugal force causes larger or denser particles to be subjected to greater force, thus being thrown to the outside of the centrifuge tube; while smaller or less dense particles are subjected to less force and remain on the inside of the centrifuge tube or closer to the center. In this way, different emulsion components are separated into layers under the action of centrifugal force.

[0048] The magnitude of the relative centrifugal force is related to the radius of rotation of its location and the rotational speed of the turntable, and its calculation formula is as follows: ; Where: RCF represents relative centrifugal force, expressed as a multiple of gravitational acceleration (g). R represents the radius of rotation, in centimeters (cm). rpm represents the rotational speed, in revolutions per minute. See the schematic diagram below. Figure 3 As shown.

[0049] Grayscale images are created after the emulsion has been thoroughly centrifuged and separated into layers using a centrifuge (10 layers). The different layers of liquid have varying light transmittance, resulting in different depths of color. However, the projected color in the cuvette changes during emulsification. To avoid experimental errors, images of different color depths can be uniformly converted to grayscale images, and the differences in grayscale color are analyzed to characterize the emulsification effect. The relationship between centrifugal force, grayscale value, and oil content of the emulsion, as determined by data testing, is as follows: Figure 4 As shown.

[0050] Analysis of the above figure shows that there is a relatively stable linear relationship between the magnitude of centrifugal force and the measured gray value and the stability of the emulsion, which confirms the rationality of the gray value method.

[0051] For the parts not covered in the above methods, existing technologies can be adopted or referenced.

[0052] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the technical solutions of the present invention, and these modifications or equivalent substitutions cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.

Claims

1. An apparatus for determining the emulsion strength stability of an emulsion, characterized in that: The system includes a centrifuge and a computer connected to the centrifuge. Inside the centrifuge is a centrifuge tube rack with several specially designed test tubes. The test tubes are connected to the centrifuge tube rack via a vertical rotation structure. The test tubes are equipped with a magnetic attraction transmission structure for magnetic fixation and data transmission. Each test tube includes a tube body, inside which are installed a light source for emitting light, a light intensity sensor for receiving light intensity data transmitted through the emulsion, and a grayscale sensor for receiving grayscale data of the emulsion after being irradiated by light.

2. The apparatus for determining the emulsion strength stability of an emulsion according to claim 1, characterized in that: The vertical rotation structure includes several fixing components for fixing specially designed test tubes, with both ends of the fixing components rotatably connected to the centrifuge tube rack.

3. The apparatus for determining the emulsion strength stability of an emulsion according to claim 2, characterized in that: The centrifuge tube rack has an opening for accommodating specially designed test tubes after vertical rotation.

4. The apparatus for determining the emulsion strength stability of an emulsion according to claim 2, characterized in that: The magnetic transmission structure includes a magnetic protrusion on a specially designed test tube, a magnetic groove on a fixing component that matches the magnetic protrusion, and metal contacts for data transmission on the magnetic protrusion and magnetic groove.

5. The apparatus for determining the emulsion strength stability of an emulsion according to claim 4, characterized in that: The magnetic transmission structure achieves power supply and data transmission through a slip ring structure.

6. The apparatus for determining the emulsion strength stability of an emulsion according to claim 1, characterized in that: The light source is located at the center inside the test tube.

7. The apparatus for determining the emulsion strength stability of an emulsion according to claim 1, characterized in that: Both the light intensity sensor and the grayscale sensor are arranged evenly in a circle on the inner wall of the test tube.

8. A test method for determining the emulsion strength stability of an emulsion, characterized in that: The apparatus for determining the emulsion strength stability of an emulsion according to any one of claims 1-7 comprises the following steps: Step 1: Take the emulsion in its natural state and pour an equal amount into a special test tube; Step two: Insert the special test tubes into the centrifuge tube rack of the centrifuge and secure them magnetically; Step 3: Turn on the computer, analyze and record the initial images, and adjust the light intensity of the light source in the test tube using computer control. Step 4: Turn on the centrifuge and perform an initial rotation test; Step 5: Once everything is ready, turn the centrifuge on full speed, set the rotation speed, and conduct a test for the specified time. Step 6: The light intensity sensor and grayscale sensor collect light intensity data and grayscale data respectively and transmit them to the computer in real time. The computer's decision-making and image display are viewed, the final result and time of emulsion stratification are recorded, and the change pattern of the image is analyzed. Step 7: Once the computer display stops changing or the predetermined time has elapsed, turn off the centrifuge.

Citation Information

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