CN-116577006-B - Multidimensional visual microscopic acting force measuring device and measuring method

CN116577006BCN 116577006 BCN116577006 BCN 116577006BCN-116577006-B

Abstract

The invention relates to a multidimensional visual microscopic acting force measuring device and a measuring method, and relates to the technical field of experimental measuring devices. The high-pressure reaction device comprises a high-pressure reaction cavity, a three-dimensional mobile table, mobile end glass fibers, fixed end glass fibers and an image and data acquisition system, wherein the mobile end glass fibers are fixed on the three-dimensional mobile table, the fixed glass fibers are fixed on the inner wall of the high-pressure reaction cavity, a first observation window is arranged at the top of the high-pressure reaction cavity, a second observation window is arranged on one side of the high-pressure reaction cavity, and the image and data acquisition system is used for measuring microcosmic acting forces in two forms of hydrate particles-hydrate particles and hydrate particles-liquid drops-wall surfaces. The invention can accurately measure the microscopic acting force among hydrate particles, liquid drops and wall surfaces of a high-pressure gas leading system through multidimensional and multi-view observation, thereby evaluating the effects of the double-effect inhibitor on preventing particle aggregation and preventing particle tube wall adhesion.

Inventors

WANG ZHIYUAN
Pei Jihao
QIN XUWEN
LU CHENG
MA CHAO
ZHANG JIANBO
LI PENGFEI

Assignees

中国石油大学(华东)
广州海洋地质调查局

Dates

Publication Date: 20260508
Application Date: 20230518

Claims (8)

1. The multidimensional visual microscopic acting force measuring device is characterized by comprising a high-pressure reaction cavity, a three-dimensional moving table, a moving end glass fiber, a fixed end glass fiber and an image and data acquisition system; the three-dimensional moving table is arranged in the high-pressure reaction cavity and can realize xyz three-dimensional movement, the movable end glass fiber is fixed on the three-dimensional moving table, the fixed end glass fiber is fixed on the inner wall of the high-pressure reaction cavity and corresponds to the position of the movable end glass fiber, the top of the high-pressure reaction cavity is provided with a first observation window, one side of the high-pressure reaction cavity is provided with a second observation window, and the image and data acquisition system is used for judging whether a research object is positioned on the same horizontal line or vertical line, accurately observing the hydrate generation form in a visual field blind area and judging whether the current particle can meet experimental requirements or not, and finally realizing the measurement of two microscopic acting forces between hydrate particle-hydrate particle and hydrate particle-liquid drop-wall surface; The image and data acquisition system comprises a first microscopic observation mirror, a second microscopic observation mirror, a pressure sensor, a temperature sensor and a data acquisition terminal, wherein the first microscopic observation mirror is vertically aligned with a first observation window, the measurement process is observed from a overlook angle, the second microscopic observation mirror is vertically aligned with a second observation window, and the measurement process is observed from a side view angle, so that multidimensional visual measurement is realized in the experimental process; The fixed form of the movable end glass fiber is divided into a horizontal fixed form and a vertical fixed form according to different measured objects, the horizontal fixed form is a movable end glass fiber I which is mainly used for measuring acting force among hydrate particles, the vertical fixed form is a movable end glass fiber II which is mainly used for measuring acting force among hydrate particles, liquid drops and wall surfaces, the moving direction of the wall surfaces is a z direction, and a side view angle is perpendicular to the moving direction of the wall surfaces, so that displacement of fixed end particles can be observed, and further microcosmic acting force among the hydrate particles, liquid drops and the wall surfaces can be calculated.
2. The multi-dimensional visual microscopic acting force measuring device according to claim 1, wherein three sides of the high-pressure reaction chamber are respectively provided with a three-dimensional moving shaft connecting rod, and one end of the three-dimensional moving shaft connecting rod extending into the high-pressure reaction chamber is connected with the three-dimensional moving table and used for driving the three-dimensional moving table to realize xyz three-dimensional movement.
3. The apparatus of claim 1, wherein the first viewing window and the second viewing window are each comprised of two glass windows, the inner glass window is made of sapphire plate, and the outer glass window is made of organic glass.
4. The multi-dimensional visual microscopic acting force measuring device according to claim 1, further comprising an air inlet system, wherein the air inlet system comprises a high-pressure air source and an air path cooling coil, the high-pressure air source is connected with the high-pressure reaction cavity through the air path cooling coil, and a pressure gauge is arranged on a pipeline for communicating the high-pressure air source with the air path cooling coil.
5. The multi-dimensional visual microscopic acting force measuring device according to claim 1, further comprising a low-temperature water bath system, wherein the low-temperature water bath system comprises a low-temperature water bath tank, ethylene glycol antifreeze is filled in the low-temperature water bath tank, the low-temperature water bath tank is connected with an outer jacket of the high-pressure reaction chamber through a hose, and the circulating pump is used for circulating the antifreeze between the low-temperature water bath tank and the outer jacket so as to maintain the experimental temperature in the high-pressure reaction chamber.
6. A method of measuring a multi-dimensional visualized micro-force, characterized by being implemented by a multi-dimensional visualized micro-force measuring device according to any one of claims 1-5, comprising the steps of: (1) The experimental preparation stage comprises the steps of reducing the temperature of a high-pressure reaction cavity to-7 to-10 ℃ by utilizing a low-temperature water bath system, selecting and measuring the elastic coefficients of two glass fibers, preparing ice particles containing double-effect inhibitor at the tip of the fixed-end glass fiber by utilizing liquid nitrogen, preparing the ice particles or placing carbon steel with liquid drops at the tip of the movable-end glass fiber, fixing the fixed-end glass fiber with the ice particles in a kettle body at the fixed end, fixing the movable-end glass fiber with the ice particles/carbon steel on a three-dimensional movable table in the high-pressure reaction cavity, and rapidly sealing the kettle body; (2) Opening an air vent valve to vacuumize the inside of a high-pressure reaction cavity, slowly adding methane into the high-pressure reaction cavity by a high-pressure gas source through a gas circuit cooling coil, closing the high-pressure gas source and the gas circuit cooling coil after the preset experimental pressure is reached, heating the temperature in the high-pressure reaction cavity to-1 ℃, heating the temperature of the high-pressure reaction cavity to 1.7 ℃, melting ice particles in the process, and generating hydrate particles under the action of high-pressure methane gas; (3) The adhesive force testing stage comprises the steps of controlling a three-dimensional moving table to move along xyz three-dimensionally by three-dimensional moving shaft connecting rods to enable an object to be tested at a moving end and the center of fixed end hydrate particles to be located on the same horizontal line or the same vertical line, controlling the three-dimensional moving shaft connecting rods to enable the object to be tested at a uniform speed to be close to the fixed end hydrate particles, enabling the moving end to press the fixed end to displace by 0.3mm after the two objects are contacted, slowly pulling away at a uniform speed after the two objects are contacted for 10 seconds, shooting a separation process of the two objects in real time by using an image and data acquisition system, converting the displacement of the fixed end into actual displacement, solving micro acting force by using Hooke's law, correcting by using a blending radius, and taking an average value of a measured result; (4) And (3) after the experiment is finished, pressure is relieved by using a vent valve.
7. The method for measuring the multidimensional visual microscopic acting force according to claim 6, wherein in the experiment preparation stage, a vacuum pump is used for vacuumizing the inside of the high-pressure reaction chamber by opening the vent valve, the pressure sensor is used for reading the pressure in the high-pressure reaction chamber, when the pressure is stabilized to be more than-0.008 MPa for 10min, the sealing performance of the chamber is good, the vent valve is closed, and a formal experiment is started.
8. The method for measuring the microscopic forces in a multi-dimensional visual manner according to claim 6, wherein the method for judging whether the centers of the objects to be measured are located on the same horizontal line or vertical line is as follows: if the movable end is a hydrate particle, the movable end and the fixed end displace in the x direction, so that the centers of the movable end hydrate particle and the fixed end hydrate particle are positioned on the same horizontal line, and the process is judged through a side view angle of the second observation window, and whether the movable end glass fiber and the fixed end glass fiber are completely overlapped is judged as a standard; If the movable end is a liquid drop-wall surface, the movable end and the fixed end displace in the z direction, so that the centers of the liquid drop-wall surface of the movable end and the hydrate particles of the fixed end are positioned on the same vertical line, and the process is judged through the depression angle of the first observation window, and the judgment standard is whether the glass fiber of the movable end and the glass fiber of the fixed end are completely overlapped.

Description

Multidimensional visual microscopic acting force measuring device and measuring method Technical Field The invention relates to the technical field of experimental measurement devices, in particular to a multidimensional visual microscopic acting force measurement device and a measurement method. Background Natural gas hydrate is a non-stoichiometric cage-like crystal formed by small molecular gas and water, has huge resource amount, is generally present in deep sea shallow stratum or frozen soil layer, and is considered as important successor energy in 21 st century. However, in deep water oil gas development and submarine pipeline transportation, natural gas and water produced by the stratum can also generate hydrates in a submarine low-temperature high-pressure environment, and the hydrates are transported, deposited and attached to the pipe wall in the pipeline through fluid carrying, so that the pipeline flow area is reduced, even a pit shaft or the pipeline is completely blocked, and serious economic loss is caused. The problem of hydrate flow assurance has restricted the great difficulty of safe and efficient development and transportation of deep water oil gas. The existing common hydrate control means mainly comprises the step of injecting thermodynamic inhibitor excessively to enable a shaft or a gathering and transportation pipeline to be completely separated from a hydrate generation area, however, the method has the advantages of large inhibitor dosage, generally more than 50wt%, high cost, high toxicity of methanol chemical agents, easy serious environmental protection problem, and difficulty in application of widely studied kinetic inhibitors in a deep sea submarine environment due to intolerance to high supercooling degree conditions. The hydrate risk management strategy which is gradually accepted in the field in recent years, allows the generation of hydrate by low-dose inhibitors such as polymerization inhibitors (0.5-2wt%) but prevents the aggregation among particles and the adhesion of pipe walls, so that the hydrate is dispersed in a continuous phase, and the method not only prevents the aggregation of the hydrate to block the pipeline, but also can improve the conveying capacity of the pipeline by forming the hydrate, thus becoming a research hot spot for students. However, the evaluation method of the double-effect hydrate inhibitor is limited, and only can be used for macroscopic evaluation through a high-pressure reaction kettle or a flow loop experiment, and the double-effect performance of the inhibitor in the aspect of inhibiting particle aggregation and preventing particle adhesion cannot be evaluated microscopically. At present, scholars propose to measure the acting force between hydrate particles and hydrate particles through a microscopic acting force measuring device (MMF) so as to visually represent the performance of a polymerization inhibitor, but the problems are that the device can only conduct one-dimensional observation, so that particles to be measured are easily not on the same horizontal line in the measuring process, the adjustment is judged according to whether two particles can be focused clearly at the same time, the device can only conduct one-dimensional observation, the hydrate particle generation form at the opposite visual angle cannot be observed, if the hydrate particles are crushed in the generating process, the particle surfaces are not smooth, the one-dimensional observation cannot be observed, experiments are conducted, the contact between measured objects is insufficient, and meanwhile, the conventional device is simply applied to the measuring of the acting force of particles, liquid drops to be measured, and the like easily occur due to gravity deformation. The above problems all cause a great measurement error. In view of the foregoing, there is a need for a microscopic force measurement device that can be visualized in multiple dimensions, and that improves upon existing measurement devices to meet the microscopic evaluation test function of "dual-effect" inhibitors. Disclosure of Invention The invention aims to provide a multidimensional visual microscopic acting force measuring device and a measuring method, which can accurately measure microscopic acting forces among hydrate particles, liquid drops and wall surfaces of a high-pressure gas leading system through multidimensional and multi-view observation, so as to evaluate the effects of a double-effect inhibitor on preventing particle aggregation and particle tube wall adhesion. The invention provides a multi-dimensional visual microscopic acting force measuring device which comprises a high-pressure reaction cavity, a three-dimensional moving table, a moving end glass fiber, a fixed end glass fiber and an image and data acquisition system, wherein the three-dimensional moving table is arranged in the high-pressure reaction cavity and can realize xyz three-dimensional movement, the moving