Spraying system for testing growth microstructure of hydrate in inhibitor-containing liquid drop and application of spraying system
By designing a spray system for testing the microscopic morphology of hydrate growth in droplets containing inhibitors, the problem of hydrate blockage in deep-sea oil and gas transportation is solved, and the precise study of hydrate generation characteristics is achieved, which is of great significance to guide the flow guarantee of oil and gas transportation pipelines.
Patent Information
- Application Number
- CN202510457875.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-14
- Publication Date
- 2025-06-13
AI Technical Summary
During the deep-sea oil and gas transportation process, hydrate blockages are prone to occur in the seabed mixed transportation pipeline, resulting in flow security problems. Especially in areas rich in moisture, it is difficult for the prior art to effectively study the microgrowth and morphology of hydrates.
A spray system was designed to test the microscopic morphology of hydrate growth in droplets containing inhibitors, including a microsampler, an automatic microscopic operating arm and a small spray can. The droplets were suspended in the oil phase through spray technology and real-time observations were performed using a cryogenic reaction table and microscope equipment.
This system can effectively simulate the growth of natural gas hydrates in oil and gas transportation pipelines, overcome the problem of insoluble in the oil phase of hydrate kinetic inhibitors, realize the precise study of hydrate generation characteristics, and is of great significance to guide the flow guarantee of oil and gas transportation pipelines.
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Figure CN120142170A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of oil and gas pipeline flow assurance, and specifically to a spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets and its application. Background Technique
[0002] China has a relatively high degree of dependence on foreign oil and gas resources. Therefore, the development and transportation of domestic oil and gas resources have always been the research focus of many scholars.
[0003] However, with the gradual depletion of onshore oil and gas resources in China, the exploitation areas of these resources are gradually moving from land to the deep sea. The environment faced during exploitation and transportation is more severe, and the engineering and technical problems to be solved are more difficult. In the actual deep-sea oil and gas transportation process, the multiphase mixed transportation pipeline technology is economically superior to single transportation. However, in the environment of low temperature, high pressure, and multiple disturbances in subsea mixed transportation pipelines, hydrates are prone to block the pipeline, bringing huge challenges to the flow assurance problem. Especially in water-rich areas such as offshore, deep sea, and permafrost, the situation where the fluid in the multiphase mixed transportation pipeline is a high-water-content system occurs frequently.
[0004] In the face of the above problems, many scholars at home and abroad have carried out a large number of studies on the prevention and control of hydrates in oil and gas pipelines. In macroscopic experiments, the experimental results are affected by many relevant factors in the reaction system, including internal temperature and pressure conditions and external mechanical structures, etc. Therefore, the experimental data is still limited and may not be universal. For microscopic experiments, it is possible to study the intrinsic kinetic laws of microscopic particles and may have statistical significance. Theoretically, the growth kinetics of hydrate crystals, especially the nucleation growth and changes in their appearance morphology of hydrates, can be studied and observed through microscopic equipment. Studying the growth and morphological properties of hydrates is of great significance for studying the formation kinetics of the overall structure of hydrates and the flow risk regulation of hydrates.
[0005] However, at present, most microscopic experimental studies focus on the effect of anti-aggregation agents on the flow aggregation of hydrates in oil-water systems, evaluate the flow risk through experiments, and explore the mechanism from a microscopic perspective. However, due to their water solubility limitations, kinetic inhibitors are mostly used in macroscopic experiments, and these studies are limited in practical applications. Summary of the Invention
[0006] The purpose of the present invention is to provide a spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets and its application to solve the problems raised in the above background technique.
[0007] The purpose of the present invention can be achieved by the following technical solutions:
[0008] A spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets, including a spray system and a testing system:
[0009] The spray system includes a microinjector, an automatic micromanipulation arm, and a small sprayer. The interior of the small sprayer contains a solution with 0.5 wt% inhibitor, and the small sprayer is used to eject small droplets.
[0010] A transparent tape is fixedly connected to the output end of the microinjector. A glass fiber is connected to both the lens tape and the automatic micromanipulation arm. Dispersed small droplets are suspended on the glass fiber connected to the transparent tape, and the extracted droplets are suspended on the glass fiber connected to the automatic micromanipulation arm.
[0011] Preferably, the test system includes a low-temperature reaction stage. The interior of the low-temperature reaction stage is divided into inner and outer cavities by a partition ring. The outer cavity is a circulating cold bath, and the inner cavity is an oil-phase system. The circulating cold bath is located around the oil-phase system. A transparent glass is fixedly connected to the central position at the bottom of the low-temperature reaction stage.
[0012] A computer system, an inverted microscope, a near-infrared camera, and a data acquisition instrument are arranged on the outer side of the low-temperature reaction stage. The computer system is electrically connected to the inverted microscope, the near-infrared camera, and the data acquisition instrument, and is used for real-time microscopic observation of the growth of cyclopentane hydrate during the entire experimental process, taking pictures and video analysis of the hydrate nucleation process, so as to analyze the microscopic morphological characteristics of hydrate growth in the inhibitor-containing droplets in the oil-phase system.
[0013] A light source with adjustable brightness is arranged on the inverted microscope. The light emitted by the light source can pass through the transparent glass and is used for supplementary lighting inside the oil-phase system.
[0014] Preferably, a temperature sensor is connected to the data acquisition instrument. The temperature sensor is arranged inside the oil-phase system and is used for collecting the temperature data inside the oil-phase system.
[0015] Preferably, a micromechanical force arm joystick and a manual micromanipulation arm are arranged on the outer side of the low-temperature reaction stage. The micromechanical force arm joystick is electrically connected to the automatic micromanipulation arm and is used for controlling the automatic micromanipulation arm. Glass fibers are connected to both the automatic micromanipulation arm and the manual micromanipulation arm, and droplets after freezing to form ice particles are on the glass fibers.
[0016] Preferably, a water bath temperature control device is arranged on the outer side of the low-temperature reaction stage. The water bath temperature control device is connected to the circulating cold bath.
[0017] A spray method for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets includes the following steps:
[0018] S1. Turn on the computer system, the data acquisition instrument, the program-controlled water bath, and the inverted microscope. Adjust the water bath temperature control device to keep the temperature sensor constant at 3.2 °C. Configure the oil-phase system and pour it into the low-temperature reaction cold stage.
[0019] S2. Weigh an appropriate amount of the hydrate kinetic inhibitor and add it to a beaker containing deionized water to prepare an aqueous solution containing 0.5 wt% of the hydrate kinetic inhibitor. Then, stir the solution for 30 minutes at a stirring rate of 650 rpm to ensure that the kinetic inhibitor is completely dissolved in the deionized water.
[0020] S3. Pour the prepared aqueous solution into a small spray bottle and shake it well. Use transparent tape to stick a longer glass fiber to the tip of the needle at the end of the microsyringe, and adjust its length to make the glass fiber slightly bent. At the same time, insert a shorter glass fiber into the end of the automatic micromanipulation arm, and use scissors to cut the glass fiber to 2 - 4 mm.
[0021] S4. Place the nozzle of the small spray bottle above the microsyringe obliquely so that the spray falls obliquely after being ejected. Some of the small droplets ejected from the spray will hang on the glass fiber of the microsyringe. Then, pick up the automatic micromanipulation arm and use the glass fiber at the end to extract the small droplets. The extraction direction can be from left to right or from right to left to make the small droplets aggregate into droplets of the required size. At the same time, the position of the droplets on the glass fiber can be adjusted, and then the glass fibers are separated.
[0022] S5. Quickly place the glass fiber with droplets in the automatic micromanipulation arm into liquid nitrogen for quenching for 10 s to ensure that the droplets are frozen to form ice particles. Then, transfer it into the oil phase system of the low-temperature reaction cold stage when it has not completely melted and there are still a small amount of ice nuclei remaining, and fix the automatic micromanipulation arm.
[0023] S6. Adjust through the micromechanical force arm joystick to make the droplets in the automatic micromanipulation arm clearly appear within the visible range of the inverted microscope.
[0024] S7. Turn on the water bath temperature control device and control the internal temperature of the circulating cold bath as follows: After stabilizing at 3.2 °C for 2 minutes, cool it at a rate of 1 °C / min to about -19.0 °C, and then immediately heat it to about 3.2 °C. At the same time, turn on the inverted microscope, near-infrared camera, and data acquisition instrument to record the changes in the growth micro-morphology during the hydrate nucleation process.
[0025] Preferably, in step S1, the configured oil phase system is 20 ml of 80% cyclopentane plus 20% n-decane.
[0026] Preferably, in step S4, the number of sprays can be controlled according to the size of the small droplets until small droplets of 0.1 - 0.5 mm 3 are ejected.
[0027] Preferably, a spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets is applied in the flow assurance of oil and gas pipelines. When the spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets is applied in the flow assurance of oil and gas pipelines, the following steps are included:
[0028] S100. Prepare an aqueous solution containing 0.5 wt% of a hydrate kinetic inhibitor and place it in a small spray bottle. Use the spray technique to suspend the inhibitor-containing droplets on the glass fiber of the micromanipulator arm, then quench them in liquid nitrogen to form ice particles, and finally quickly place them in the oil phase of the cold stage.
[0029] S200. Adjust the hydrate particles suspended at the end of the micromanipulator arm to the visible range of the inverted microscope through the micromechanical force arm joystick.
[0030] S300. Turn on the near-infrared camera and the inverted microscope to record videos, turn on the water bath temperature control device to control the temperature, and record the changes in the microscopic morphology during the hydrate formation process.
[0031] Advantages of the present invention:
[0032] (1) The device is simple and easy to operate. The data acquisition system and the image processing system can very intuitively observe the influence of the inhibitor on the dynamic growth morphology of hydrates.
[0033] (2) Through the spray technique, the problem of how to smoothly place the droplets in the oil phase and observe them is effectively solved.
[0034] (3) It overcomes the problem that the hydrate kinetic inhibitor is insoluble in the oil phase, making it difficult to measure the influence of the inhibitor on the formation of hydrates in water droplets in the oil phase. Description of the drawings
[0035] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, for those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings;
[0036] Figure 1 is a schematic structural diagram of the spray system proposed by the present invention;
[0037] Figure 2 is a schematic structural diagram of the test system proposed by the present invention.
[0038] The reference numerals in the drawings are as follows:
[0039] 1. Near-infrared camera; 2. Computer system; 3. Automatic micromanipulation arm; 4. Manual micromanipulation arm; 5. Micromechanical force arm joystick; 6. Inverted microscope; 7. Low-temperature reaction cold stage; 8. Oil phase system; 9. Transparent glass; 10. Water bath temperature control equipment; 11. Circulating cold bath; 12. Data acquisition instrument; 13. Temperature sensor; 14. Glass fiber; 15. Droplet; 16. Light source; 17. Microsyringe; 18. Transparent tape; 19. Small sprayer; 20. Spray; 21. Small droplet. Detailed implementation mode
[0040] The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
[0041] A spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets, including a spray system and a test system:
[0042] The spray system includes a microsyringe 17, an automatic micromanipulation arm 3 and a small sprayer 19. The solution contained in the small sprayer 19 is an aqueous solution containing 0.5 wt% of a hydrate kinetic inhibitor, and the small sprayer 19 is used to spray small droplets 21;
[0043] The output end of the microsyringe 17 is fixedly connected with a transparent tape 18. A glass fiber 14 is connected to both the lens tape 18 and the automatic micromanipulation arm 3. Dispersed small droplets 21 are suspended on the glass fiber 14 connected to the transparent tape 18, and the extracted droplet 15 is suspended on the glass fiber 14 connected to the automatic micromanipulation arm 3.
[0044] The length of the glass fiber 14 can be cut. The glass fiber 14 adhered to the microsyringe 17 is generally longer (20 - 30 mm); the glass fiber 14 inserted into the micromanipulation arm is shorter (2 - 4 mm);
[0045] A longer glass fiber 14 is wound around the microsyringe 17 through the transparent tape 18 to facilitate the suspension of small inhibitor-containing droplets, and then the automatic micromanipulation arm 3 is used to collect a droplet of a suitable size ().
[0046] The test system includes a low-temperature reaction stage 7. The interior of the low-temperature reaction stage 7 is divided into inner and outer cavities through a partition ring. The outer cavity is a circulating cold bath 11, and the inner cavity is an oil phase system 8. The circulating cold bath 11 is located around the oil phase system 8. The center position at the bottom of the low-temperature reaction stage 7 is fixedly connected with a transparent glass 9;
[0047] Outside the low-temperature reaction stage 7, there are a computer system 2, an inverted microscope 6, a near-infrared camera 1, and a data acquisition instrument 12. The computer system 2 is electrically connected to the inverted microscope 6, the near-infrared camera 1, and the data acquisition instrument 12, and is used to microscopically observe the growth of cyclopentane hydrate in real time during the entire experimental process, take pictures and conduct video analysis of the hydrate nucleation process, so as to analyze the microscopic morphological characteristics of hydrate growth in the inhibitor-containing droplets in the oil phase system;
[0048] The computer system 2 is equipped with SimplePIC image processing software. In the computer system 2, the SimplePCI software can be used to observe the morphological changes of cyclopentane hydrate during the entire experimental process with the near-infrared camera, and take pictures and videos, and the obtained images can be observed, recorded, and processed in real time.
[0049] The model of the inverted microscope 6 is Carl Zeiss Axio Observer A1, and the magnification of the eyepiece used in the experiment is 5 times.
[0050] The model of the data acquisition instrument 12 is Agilent 34970A, in which a thermocouple is set as the temperature sensor, which is used to measure the change of the oil phase temperature during the formation of cyclopentane hydrate.
[0051] On the inverted microscope 6, there is a light source 16 whose brightness can be controlled. The light emitted by the light source 16 can pass through the transparent glass 9 and is used to supplement light inside the oil phase system 8.
[0052] A temperature sensor 13 is connected to the data acquisition instrument 12, and the temperature sensor 13 is arranged inside the oil phase system 8 and is used to collect the temperature data inside the oil phase system 8.
[0053] Outside the low-temperature reaction stage 7, there are a micro-mechanical force arm joystick 5 and a manual microscopic operation arm 4. The micro-mechanical force arm joystick 5 is electrically connected to the automatic microscopic operation arm 3 and is used to control the automatic microscopic operation arm 3. Glass fibers 14 are connected to both the automatic microscopic operation arm 3 and the manual microscopic operation arm 4, and there are droplets 15 with frozen ice particles on the glass fibers 14.
[0054] The automatic micromanipulator (Eppendorf TransferMan NK2) has a range of 0 - 2000 μm and an accuracy of 1 μm; the manual micromanipulator (3D Hydraulic Coarse / Fine Micromanipulator MWO - 202D) has a range of 0 - 1500 μm and an accuracy of 1 μm. A capillary fiber (i.e., glass fiber 14) is inserted at their ends to suspend the liquid droplet. The micromechanical force arm joystick 5 can be controlled at the micron level in four directions: up, down, left, and right. There are microscopes on both the automatic micromanipulator 3 and the manual micromanipulator 4. Using the automatic micromanipulator 3 and the manual micromanipulator 4, the microscope can be operated to focus on the liquid droplet particles so that the entire reaction process can be clearly observed in the microscopic field of view.
[0055] A water bath temperature control device 10 is provided outside the low - temperature reaction table 7, and the water bath temperature control device 10 is connected to the circulating cold bath 11.
[0056] The coolant used in the water bath temperature control device 10 is 75% ethanol. The water bath temperature control device 10 is connected to the low - temperature reaction table 7 through an external circulating cold bath 11. The coolant can be programmed to control the temperature in the water bath and then adjust the temperature of the low - temperature reaction table 7 through an external circulating pipe.
[0057] A spraying method for testing the microscopic morphology of hydrate growth in inhibitor - containing droplets includes the following steps:
[0058] S1. Turn on the computer system 2, data acquisition instrument 12, programmable water bath 10, and inverted microscope 6. Adjust the water bath temperature control device 10 to keep the temperature sensor 13 constant at 3.2 °C. Configure the oil - phase system 8 and pour it into the low - temperature reaction cold table 7.
[0059] S2. Weigh an appropriate amount of hydrate kinetic inhibitor, add it to a beaker containing deionized water, and configure an aqueous solution containing 0.5 wt% hydrate kinetic inhibitor. Then stir the solution for 30 min at a stirring rate of 650 rpm to ensure that the kinetic inhibitor is completely dissolved in deionized water.
[0060] S3. Pour the prepared aqueous solution into a small spray bottle 19 and shake it well. Use transparent tape 18 to stick a longer glass fiber 14 to the needle tip at the end of the microsyringe 17, adjust its length to make the glass fiber 14 slightly bent. At the same time, insert a shorter glass fiber 14 into the end of the automatic micromanipulator 3, and use scissors to cut the glass fiber 14 to an appropriate length (2 - 4 mm).
[0061] S4. Place the nozzle of the small spray bottle 19 above the inclined direction of the microinjector 17, so that the spray 20 falls obliquely after spraying. Some of the small droplets 21 ejected from the spray 20 will hang on the fiberglass 14 of the microinjector 17. Then pick up the automatic micromanipulator arm 3 and use the fiberglass 14 at the end to extract the small droplet 21. The extraction direction can be from left to right or from right to left, so that the small droplets 21 aggregate into droplets 15 of the required size. At the same time, the position of the droplet 15 on the fiberglass 14 can be adjusted, and then the fiberglass 14 is separated.
[0062] S5. Quickly place the fiberglass 14 with the droplet 15 in the automatic micromanipulator arm 3 into liquid nitrogen for quenching for 10 s to ensure that the droplet 15 freezes to form ice particles. Immediately transfer it into the oil phase system 8 of the low-temperature reaction cold stage 7 when it has not completely melted and there are still a small number of ice nuclei remaining, and fix the automatic micromanipulator arm 3.
[0063] S6. Adjust through the micromachinery force arm joystick 5 so that the droplet 15 in the automatic micromanipulator arm 3 clearly appears within the visible range of the inverted microscope 6.
[0064] S7. Turn on the water bath temperature control device 10 and control the internal temperature of the circulating cold bath 11: After stabilizing at 3.2 °C for 2 min, cool down at a rate of 1 °C / min to about -19.0 °C, and then immediately heat up to about 3.2 °C. At the same time, turn on the inverted microscope 6, the near-infrared camera 1, and the data acquisition instrument 12 to record the changes in the growth micro-morphology during the hydrate nucleation process.
[0065] In the step S1, the configured oil phase system 8 is 20 ml of 80% cyclopentane plus 20% n-decane.
[0066] In the step S4, the number of sprays can be controlled according to the size of the small droplets 21 until small droplets of 0.1 - 0.5 mm 3 are ejected.
[0067] The application of a spray system for testing the growth micro-morphology of hydrates in inhibitor-containing droplets in the flow assurance of oil and gas pipelines. When the spray system for testing the growth micro-morphology of hydrates in inhibitor-containing droplets is applied in the flow assurance of oil and gas pipelines, the following steps are included:
[0068] S100. After preparing an aqueous solution containing 0.5 wt% of a hydrate kinetic inhibitor and placing it in the small spray bottle 19, use the spraying technique to suspend the inhibitor-containing droplets on the fiberglass 14 of the micromanipulator arm. Then quench them in liquid nitrogen to form ice particles, and finally quickly place them in the oil phase of the cold stage.
[0069] S200. Adjust the hydrate particles suspended at the end of the micromanipulator arm to the visible range of the inverted microscope through the micromachinery force arm joystick 5.
[0070] Turn on the near-infrared camera 1 and the inverted microscope 6 to record videos, turn on the water bath temperature control device 10 to control the temperature, and record the changes in the growth micro-morphology during the formation of hydrates.
[0071] The present invention can simulate the growth of natural gas hydrates in oil and gas transportation pipelines, and use the combination of spray technology and microscopic observation means to study the nucleation and micro-morphology of natural gas hydrates, effectively solving the problem of the use of hydrate kinetic inhibitors in the oil phase system at the laboratory small-scale test level, thereby accurately studying the formation characteristics of natural gas hydrates, which has certain guiding significance for oil and gas transportation pipelines.
[0072] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments, and what is described in the above embodiments and the specification only illustrates the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements all fall within the scope of the present invention claimed.
Claims
1. A spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets, characterized in that: Including spray system and test system: The spray system includes a micro-injector (17), an automatic micromanipulator arm (3) and a small spray pot (19), wherein the small spray pot contains a solution containing 0.5 wt% of an inhibitor, and the small spray pot (19) is used to spray small droplets (21); The output end of the micro-injector (17) is fixedly connected to a transparent tape (18); a glass fiber (14) is connected to the lens tape (18) and the automatic micromanipulation arm (3); dispersed small droplets (21) are suspended on the glass fiber (14) connected to the transparent tape (18); and extracted droplets (15) are suspended on the glass fiber (14) connected to the automatic micromanipulation arm (3).
2. A spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets according to claim 1, characterized in that: The test system comprises a low temperature reaction table (7), wherein the interior of the low temperature reaction table (7) is divided into inner and outer cavities by a separation ring, wherein the outer cavity is a circulating cold bath (11), and the inner cavity is an oil phase system (8), wherein the circulating cold bath (11) is located around the oil phase system (8), and a transparent glass (9) is fixedly connected to the center of the bottom of the low temperature reaction table (7); A computer system (2), an inverted microscope (6), a near-infrared camera (1) and a data acquisition device (12) are arranged outside the low-temperature reaction table (7). The computer system (2) is electrically connected to the inverted microscope (6), the near-infrared camera (1) and the data acquisition device (12) to observe the growth of cyclopentane hydrate in real time during the entire experiment, take photos and record videos of the hydrate nucleation process, and analyze the microscopic morphological characteristics of the hydrate growth in the inhibitor-containing droplets in the oil phase system.
3. A spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets according to claim 2, characterized in that: The inverted microscope (6) is provided with a light source (16) with controllable brightness. The light emitted by the light source (16) can pass through the transparent glass (9) and is used to provide supplementary light for the interior of the oil phase system (8).
4. A spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets according to claim 2, characterized in that: The data acquisition instrument (12) is connected to a temperature sensor (13), which is arranged inside the oil phase system (8) and is used to collect temperature data inside the oil phase system (8).
5. A spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets according to claim 2, characterized in that A micromechanical lever (5) and a manual micromanipulation arm (4) are arranged on the outer side of the low-temperature reaction table (7); the micromechanical lever (5) and the automatic micromanipulation arm (3) are electrically connected to control the automatic micromanipulation arm (3); the automatic micromanipulation arm (3) and the manual micromanipulation arm (4) are both connected to glass fibers (14); and liquid droplets (15) formed by freezing to generate ice particles are disposed on the glass fibers (14).
6. A spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets according to claim 2, characterized in that: A water bath temperature control device (10) is arranged outside the low-temperature reaction table (7), and the water bath temperature control device (10) is connected to a circulating cold bath (11).
7. A spray method for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets, characterized in that: The following steps are involved: S1, turn on the computer system (2), the data acquisition instrument (12), the program-controlled temperature water bath (10) and the inverted microscope (6), adjust the water bath temperature control device (10) to make the temperature sensor (13) constant at 3.2°C, prepare the oil phase system (8), and pour it into the low-temperature reaction cold stage (7); S2. Weigh an appropriate amount of hydrate kinetic inhibitor and add it into a beaker containing deionized water to prepare an aqueous solution containing 0.5 wt % of the hydrate kinetic inhibitor. Then stir the solution for 30 min at a stirring rate of 650 rpm to ensure that the kinetic inhibitor is completely dissolved in the deionized water. S3, pour the prepared aqueous solution into a small spray bottle (19) and shake it well, use transparent tape (18) to stick a longer glass fiber (14) to the needle at the end of the microinjector (17), adjust its length so that the glass fiber (14) is slightly bent, and at the same time, insert a shorter glass fiber (14) into the end of the automatic micromanipulator arm (3), and use scissors to cut the glass fiber (14) to 2-4 mm; S4, placing the nozzle of the small spray pot (19) above the micro-injector (17) obliquely, so that the spray (20) falls in an oblique direction after being sprayed out, and the small droplets (21) sprayed out by part of the spray (20) will be suspended on the glass fiber (14) of the micro-injector (17), and then the automatic micromanipulator arm (3) is picked up, and the glass fiber (14) at the end is used to extract the small droplets (21), and the extraction direction can be from left to right or from right to left, so that the small droplets (21) are gathered into droplets (15) of a desired size, and the position of the droplets (15) on the glass fiber (14) can be adjusted at the same time, and then the glass fiber (14) is separated; S5, quickly placing the glass fiber (14) with the liquid droplet (15) in the automatic micromanipulator arm (3) into liquid nitrogen for quenching (10) seconds, ensuring that the liquid droplet (15) is frozen to form ice particles, and then transferring it into the oil phase system (8) of the low-temperature reaction cold stage (7) when it is not completely melted and a small amount of ice nuclei remain, and fixing the automatic micromanipulator arm (3); S6. The micromechanical arm joystick (5) is adjusted so that the droplet (15) in the automatic micromanipulation arm (3) appears clearly within the visible range of the inverted microscope (6). S7. Turn on the water bath temperature control device (10) to control the internal temperature of the circulating cold bath (11): after stabilizing at 3.2°C for 2 minutes, cool down to about -19.0°C at a rate of 1°C / min, and then immediately heat up to about 3.2°C. At the same time, turn on the inverted microscope (6), near-infrared camera (1), and data acquisition instrument (12) to record the growth micromorphology changes during the hydrate nucleation process.
8. A spray method for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets according to claim 7, characterized in that: In the step S1, the oil phase system (8) is prepared by adding 80% cyclopentane and 20% n-decane, totaling 20 ml.
9. A spray method for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets according to claim 7, characterized in that: In step S4, the number of times of spraying can be controlled according to the size of the small droplets (21), until a droplet of 0.1 to 0.5 mm is sprayed. 3 until the small droplets (21) are formed.
10. A spray system for testing the microscopic morphology of hydrate growth in inhibitor-containing droplets as claimed in claim 1, used in flow assurance of oil and gas pipelines, characterized in that: When the spray system for testing the micromorphology of hydrate growth in inhibitor droplets is used in oil and gas pipeline flow assurance, the following steps are included: S100, prepare an aqueous solution containing 0.5 wt% of a hydrate kinetic inhibitor and place it in a small spray bottle (19), use a spray technique to suspend inhibitor droplets on the glass fiber (14) of a micromanipulator arm, then quench in liquid nitrogen to form ice particles, and finally quickly place them in the oil phase of a cold stage. S200, adjusting the hydrate particles suspended at the end of the micromanipulator arm to within the visible range of the inverted microscope via the micromechanical arm joystick (5). S300, turning on the near-infrared camera (1) and the inverted microscope (6) to record the video, turning on the water bath temperature control device (10) to control the temperature, and recording the growth microscopic morphology changes during the hydrate formation process.
Citation Information
Patent Citations
Device and method for research of low-dosage inhibitor of natural gas hydrate
CN102169112A
A microreactor capable of visual observation of a gas hydrate reacting process
CN105548183A
Microscopic and macroscopic evaluation method for double-effect hydrate inhibitor
CN114609337A
