CN108535180B - Device and method for measuring micro-adhesion force among hydrate particles in gas phase system - Google Patents
Device and method for measuring micro-adhesion force among hydrate particles in gas phase system Download PDFInfo
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Abstract
The invention relates to a device and a method for measuring micro-adhesion force among hydrate particles in a gas phase system, which comprises a first micro-operation system, a second micro-operation system, a visual reaction device, a photographing/video recording system, a low-temperature constant-temperature control system and a temperature acquisition instrument, wherein the first micro-operation system is connected with the second micro-operation system through a pipeline; the first microscopic operation system comprises a high-precision first three-dimensional operation platform and a first operation arm, wherein the first three-dimensional operation platform comprises a first XY operation platform and a first Z operation platform; the visual reaction device is used for generating hydrate particles; the photographing/video recording system is used for acquiring the displacement of hydrate particles in the visual reaction device; the low-temperature constant-temperature control system is used for providing stable working temperature for the visual reaction device; the temperature acquisition instrument is used for measuring the working temperature in the visual reaction device in real time. The invention provides a method for testing the micro-adhesion force among hydrate particles in a gas phase system, which can better test and analyze the micro-adhesion force among the hydrate particles in the gas phase system.
Description
Technical Field
The invention relates to an experimental device and method for micro-adhesion among hydrate particles, in particular to a device and method for measuring the micro-adhesion among hydrate particles in a gas phase system.
Background
The gas hydrate is a water molecule solid crystal with a cage structure. The structural cavities consisting of water molecules are filled with small molecules that act to stabilize the crystal lattice. Small molecules include hydrocarbons of relatively small molecular mass, such as methane, ethane, propane, as well as hydrogen and carbon dioxide. Under the condition that the deep water and ultra-deep water areas have the environmental characteristics of high pressure and low temperature, light hydrocarbon components (such as methane, ethane and the like) in the oil-gas gathering and transportation pipeline are easy to generate natural gas hydrate with water, and the normal transportation of the pipeline is seriously influenced.
In the exploration process of the hydrate pipeline plugging mechanism, the large loop test plays a key role in macroscopic exploration and qualitative cognition of the pipeline plugging mode, however, the inherent control mechanism of the hydrate pipeline plugging mode is explained, the quantitative description of the key process is realized, and the macro test is difficult to realize. Based on the method, the key acting force involved in the hydrate aggregation process is taken as a starting point, the control mechanism of hydrate aggregation can be basically clarified through systematic experimental exploration and theoretical analysis, quantitative description and evaluation are realized, and the method has great significance for risk assessment and prevention strategy formulation of hydrate generation in oil and gas gathering and transportation pipelines. However, at present, research on a hydrate blockage mechanism in a pipeline explored by a hydrate microscopic stress characteristic system is very limited, and experimental tests and theoretical research of a plurality of key mechanical parameters are still in an initial exploration stage, and particularly, the research on a gas transmission pipeline is a fresh relevant report.
The generation of gas hydrate needs to meet the conditions of low temperature and high pressure, and in the prior art, a high-pressure micro mechanical force measuring device is mainly adopted to measure the micro adhesion force among hydrate particles in a gas phase system. The whole system comprises: the high-pressure reaction tank consists of a test unit and a micro mechanical force operation unit, wherein the test unit resists high pressure of 10MPa and is provided with an air inlet and an air outlet; the pressure supply system supplies high pressure to the reaction tank through the air inlet; the temperature control system is used for controlling the temperature of the gas in the reaction tank; and the data acquisition and processing system is used for acquiring and analyzing various data of the pressure supply system, the reaction tank and the temperature control system. The whole set of device has the following problems: 1. the experiment is carried out at low temperature and high pressure, the danger coefficient is high, and the requirement on the safety performance of the device is high; 2. the device is complex, the experimental conditions are not easy to control, and the operability is low; 2. the equipment is expensive and cannot be generally applied to the research of the micro-adhesion force among the hydrate particles of the gas phase system.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a device for measuring the microscopic adhesion force among hydrate particles in a gas phase system;
the invention also provides a method for measuring the micro-adhesion among hydrate particles in the gas phase system;
interpretation of terms:
1. the micro-adhesion force between hydrate particles refers to the force of the hydrate particles adhering to the surface of another hydrate particle after the hydrate particles are contacted.
2. The elastic coefficient of the glass fiber is the ratio of the stress to the strain to which the glass fiber is subjected.
The technical scheme of the invention is as follows:
a device for measuring the micro-adhesion force among hydrate particles in a gas phase system comprises a first micro-operation system, a second micro-operation system, a visual reaction device, a photographing/video recording system, a low-temperature constant-temperature control system and a temperature acquisition instrument;
the first microscopic operating system comprises a high-precision first three-dimensional control platform and a first operating arm clamped on the first three-dimensional control platform, the first three-dimensional control platform comprises a first XY operating platform (model LY-125-LM-50) and a first Z operating platform (model LZ125-2), and contact surfaces of the first XY operating platform and the first Z operating platform are fixedly connected through bolts;
the second microscopic operating system comprises a high-precision second three-dimensional control platform and a second operating arm clamped on the second three-dimensional control platform, and the second three-dimensional control platform comprises a second XY operating platform (model LY-125-RM-50) and a second Z operating platform (model LZ 125-2);
the first XY operating platform and the second XY operating platform are used for accurately moving the hydrate particles in the X, Y direction; the first Z operation platform and the second Z operation platform are used for enabling hydrate particles to accurately move in the Z direction; the X, Y directions refer to two directions which are vertical to each other on a horizontal plane, and the Z direction refers to a vertical direction; the first operating arm and the second operating arm are used for suspending hydrate particles;
the visual reaction device is used for generating hydrate particles; the photographing/video recording system is used for acquiring the displacement of hydrate particles in the visual reaction device; the low-temperature constant-temperature control system is used for providing stable working temperature for the visual reaction device; the temperature acquisition instrument is used for measuring the working temperature of the visual reaction device in real time.
According to the invention, the visual reaction device comprises a temperature control circulation tank, a circulation liquid inlet, a circulation liquid outlet, an operation unit and a double-layer glass window, wherein the low-temperature constant-temperature control system is respectively communicated with the temperature control circulation tank through the circulation liquid inlet and the circulation liquid outlet, the operation unit is arranged in the temperature control circulation tank, and the double-layer glass window is arranged at the position of the side surface of the operation unit corresponding to the photographing/video recording system.
The temperature control circulation tank inputs and outputs circulating liquid through a circulating liquid inlet and a circulating liquid outlet, and provides stable working temperature for the operation unit by utilizing the principle of circulating refrigeration; acquiring the displacement of hydrate particles in the operation unit by a photographing/video recording system through a double-layer glass window; the ambient air is moist, and reaction temperature is lower, and visual reaction unit's window temperature is less than the room temperature, and the surface is covered with one deck water smoke easily, adopts the double glazing window can solve this water smoke problem.
According to the invention, the device further comprises a cyclopentane micro-supply device which is communicated with the operation unit.
The operation unit is internally provided with cyclopentane which has strong volatility, and a trace cyclopentane supply device is arranged for maintaining the liquid amount in the operation unit constant, so that the problem of liquid level reduction caused by volatilization of cyclopentane is solved by utilizing the siphon principle.
According to the invention, the length of the operation unit is 3-4cm, the width of the operation unit is 3-4cm, and the height of the operation unit is 7-8 cm;
the deeper operating unit is beneficial to keeping the gas in the operating unit at a lower temperature and keeping the space near the liquid level at the bottom at a higher concentration of cyclopentane vapor.
According to the invention, the first operation arm comprises a first metal arm, a first stainless steel thin tube and first glass fiber, one end of the first metal arm is clamped on the first three-dimensional control platform, the other end of the first metal arm is welded with the first stainless steel thin tube, and the tail end of the first stainless steel thin tube is connected with the first glass fiber. The first glass fibers are used to suspend the hydrate particles.
The second operation arm comprises a second metal arm, a second stainless steel thin tube and second glass fibers, one end of the second metal arm is clamped on the second three-dimensional control platform, the other end of the second metal arm is welded to the second stainless steel thin tube, and the tail end of the second stainless steel thin tube is connected with the second glass fibers. The second glass fiber is used to suspend the hydrate particles.
According to the invention, the outer diameter of the first stainless steel thin tube is preferably 0.5-0.8mm, and the stainless steel thin tube in the outer diameter range is easy to connect the first glass fiber; the diameter of the first glass fiber is 30-50um, the adhesion force among hydrate particles is small, and the deformation of the first glass fiber with the diameter of 30-50um under the action of the adhesion force is easily obtained through a stereoscopic microscope. The outer diameter of the second stainless steel thin tube is 0.5-0.8mm, and the diameter of the second glass fiber is 50-100 um; the elastic coefficient of the second glass fiber in the diameter range is larger than that of the first glass fiber of 30-50um, so that only the first glass fiber of 30-50um in diameter is obviously deformed in the contact and separation process of hydrate particles, and the displacement of the hydrate particles can be conveniently measured.
According to the present invention, preferably, the photographing/recording system includes a stereoscopic microscope and a computer, the computer is connected to the stereoscopic microscope, and the stereoscopic microscope obtains the displacement of the hydrate particles in the operation unit through the double-layer glass window; and measuring and analyzing the adhesive force by using Hooke's law according to the elastic coefficient of the glass fiber.
According to the invention, the device further comprises a visual isolation hood, the first microscopic operation system, the second microscopic operation system, the visual reaction device, the stereoscopic microscope, the temperature acquisition instrument and the cyclopentane micro-supply device are all arranged in the visual isolation hood, and an operation window is arranged on the visual isolation hood.
The visual isolation hood isolates the microscopic operation system, the visual reaction device, the stereomicroscope, the temperature acquisition instrument and the cyclopentane micro-supply device from the external environment, reduces air flow and reduces the volatilization rate of cyclopentane; external dust and water vapor are effectively prevented from entering the operating environment, and the operating environment is kept relatively clean and dry; visual shield is equipped with the operation window, makes things convenient for the experiment operation, closes the operation window after the operation.
According to the invention, the temperature acquisition instrument comprises a digital thermometer and a probe, wherein the digital thermometer is connected with the probe, and a probe head of the probe extends into the operation unit to measure the temperature of a gas phase system near the liquid level in the operation unit in real time.
According to the invention, the low-temperature constant-temperature control system is preferably a low-temperature constant-temperature tank which is respectively connected with the circulating liquid inlet and the circulating liquid outlet through rubber pipelines.
According to the invention, the visual isolation hood is preferably made of transparent organic glass; the temperature control circulating tank is made of stainless steel; the double-layer glass window is made of high-transparency colorless glass.
The visual isolation cover is made of transparent organic glass, and the transparent organic glass can be used for conveniently observing the experimental state in the visual isolation cover; the double glazing window adopts the high glass material that passes through, realizes that the operation is visual, and the temperature control circulation groove adopts stainless steel, is convenient for control the temperature in the operating unit and increases device intensity.
The method for measuring the micro-adhesion force among hydrate particles in the gas phase system by adopting the device comprises the following steps:
A. determination of the modulus of elasticity of glass fibers
B. Producing hydrate particles in a gas phase system; the method comprises the following steps:
(1) injecting 20-30ml of cyclopentane solution (with the concentration of 96%) into the operation unit;
(2) adjusting the low-temperature constant-temperature tank to enable the temperature of a gas phase system above the liquid level of cyclopentane in the operation unit to reach (-3) - (-2);
(3) producing a droplet at the end of the first glass fiber, the droplet having a diameter d, 600um < d <700 um;
(4) putting the liquid drops into liquid nitrogen for 20-30s to manufacture first ice particles;
(5) clamping the first operating arm on the first three-dimensional operating platform, operating the first three-dimensional operating platform, and placing first ice particles at a position 3-5mm above the liquid level of cyclopentane in an operating unit;
(6) creating a droplet in the middle of the second glass fiber, the droplet having a diameter d, 600um < d <700 um; the elastic coefficient of the middle position of the glass fiber is large, so that the second glass fiber is ensured not to deform obviously in the contact and separation process of hydrate particles;
(7) putting the liquid drops into liquid nitrogen for 20-30s to manufacture second ice particles;
(8) clamping the second operating arm on the second three-dimensional operating platform, operating the second three-dimensional operating platform, and placing second ice particles at a position 3-5mm above the liquid level of cyclopentane in the operating unit;
(9) adjusting the low-temperature constant-temperature tank, increasing the temperature by 1 ℃ every 10min until the temperature of a gas phase system above the cyclopentane solution reaches 0 ℃, keeping the temperature for 30min, and waiting for the first ice particles and the second ice particles to melt to generate first hydrate particles and second hydrate particles;
C. measurement of the adhesion between hydrate particles in a gas phase System
(10) Adjusting the low-temperature constant-temperature tank to enable the temperature of a gas phase system in the operation unit to reach the experimental temperature T1，0℃<T1<7.7℃；
(11) Starting the photographing/recording system;
(12) operating the first three-dimensional control platform and the second three-dimensional control platform to enable the first hydrate particles and the second hydrate particles to be in the same vertical plane, namely, the first hydrate particles and the second hydrate particles are overlapped when the upper surface of the operation unit vertically downwards looks;
(13) operating the second three-dimensional control platform, slowly moving (9 +/-3 um/s) the second hydrate particles to contact the first hydrate particles, and applying a load △ P, wherein 2uN is more than △ P and less than 8uN, so that the first glass fibers are deformed and kept for 10 s;
(14) operating the second three-dimensional control platform, slowly moving (9 +/-3 um/s) the second hydrate particles to slowly separate the first hydrate particles from the second hydrate particles, and recording the terminal deformation displacement △ x of the first glass fiber when the two hydrate particles are just separated by using the stereoscopic microscope2The microscopic adhesion between hydrate particles is obtained by Hooke's law
Preferably, step a includes:
a. clamping a first operating arm on a first three-dimensional control platform, placing a small cone (made of polytetrafluoroethylene and providing an action point for the tail end of a glass fiber) on an objective table of a precision electronic balance, opening the precision electronic balance, and recording the reading m of the precision electronic balance1；
b. Operating the first three-dimensional control platform to enable the tail end of the first glass fiber to be just contacted with the vertex of a small cone on an objective table of the precision electronic balance;
c. operating the first Z operating platform to make the first operating arm slowly descend for 300-1And recording the reading m of the precision electronic balance2；
d. Calculating the elastic coefficient of the glass fiber
e. Repeating the steps b-d30 times or more to obtain the average value of the elastic coefficient of the glass fiber
。
The invention has the beneficial effects that:
1. according to the invention, the high-precision first three-dimensional control platform and the second three-dimensional operation platform are adopted, hydrate particles in the operation unit are allowed to accurately move in the directions of x, y and z, the displacement of the hydrate particles in the operation unit is obtained through the double-layer glass window, and the adhesion is measured and analyzed by using the Hooke's law according to the elastic coefficient of glass fibers.
2. The invention designs the cyclopentane real-time supplement system by utilizing the siphon principle, has simple operation and low manufacturing cost, solves the problem of liquid level reduction caused by volatilization of cyclopentane and keeps the amount of cyclopentane liquid in the operation unit constant.
3. The invention designs the gas phase system operation unit, which can keep the gas phase in the operation unit at lower temperature and keep the space near the liquid level at the bottom at higher concentration of cyclopentane vapor, thereby avoiding the decomposition of cyclopentane hydrate particles in the gas phase system.
4. The invention provides a method for testing the micro-adhesion force among hydrate particles in a gas phase system, which can better test and analyze the micro-adhesion force among the hydrate particles in the gas phase system.
5. The invention provides a method for measuring the elastic coefficient of glass fiber, which is simple to operate and has lower equipment cost.
6. According to the invention, cyclopentane is adopted to research the micro adhesion force among hydrate particles, so that the high-pressure and low-temperature conditions required by gas hydrate generation are avoided, the experiment can be completed under normal pressure, the whole set of device is easy to build, the system cost is low, and the safety coefficient is high.
Drawings
FIG. 1 is a structural connection diagram of an apparatus for measuring micro-adhesion between hydrate particles in a gas phase system.
FIG. 2 is a schematic view of a visual cage of the present invention.
FIG. 3 is a schematic view of an apparatus for measuring the modulus of elasticity of glass fibers according to the present invention.
FIG. 4 is a schematic representation of the procedure for measuring the micro-adhesion between hydrate particles in a gas phase system according to the present invention.
FIG. 5 shows a set of 32 measurements of the modulus of elasticity of the glass fiber on the first manipulator arm of the present invention.
FIG. 6 is a diagram showing the adhesion measurement steps taken 30min after hydrate particles were formed in the gas phase system at 1 ℃.
1. The device comprises a low-temperature constant-temperature tank, 2, a rubber pipeline, 3, a first three-dimensional control platform, 4, a computer, 5, a data line, 6, a body type microscope, 7, a first operating arm, 8, a circulating liquid inlet, 9, a double-layer glass window, 10, an operating unit, 11, a temperature control circulating tank, 12, a stainless steel thin tube, 13, a cyclopentane micro-supply device, 14, a digital thermometer, 15 and a visual isolation cover; 16. an operating window; 17. the device comprises a first XY operation platform, 18, a first Z operation platform, 19, a first metal arm, 20, a first stainless steel thin tube, 21, first glass fibers, 22, a small cone, 23, a precision electronic balance, 24, a micro-injector, 25, liquid drops, 26, liquid nitrogen, 27, a liquid nitrogen tank, 28 and cyclopentane.
Detailed Description
The invention is further defined in the following, but not limited to, the figures and examples in the description.
Example 1
A device for measuring the micro-adhesion force among hydrate particles in a gas phase system is shown in figure 1 and comprises a first micro-operation system, a second micro-operation system, a visual reaction device, a photographing/video recording system, a low-temperature constant-temperature control system and a temperature acquisition instrument;
the first microscopic operation system comprises a high-precision first three-dimensional control platform 3 and a first operation arm 7 clamped on the first three-dimensional control platform 3, the first three-dimensional control platform 3 comprises a first XY operation platform 17 (model LY-125-LM-50) and a first Z operation platform 18 (model LZ125-2), and the contact surfaces of the first XY operation platform 17 and the first Z operation platform are fixedly connected through bolts;
the second microscopic operating system comprises a high-precision second three-dimensional control platform and a second operating arm clamped on the second three-dimensional control platform, and the second three-dimensional control platform comprises a second XY operating platform (model LY-125-RM-50) and a second Z operating platform (model LZ 125-2);
the first XY operating platform 17 and the second XY operating platform are used for accurately moving the hydrate particles in the direction of X, Y; the first Z operation platform 18 and the second Z operation platform are used for enabling hydrate particles to move accurately in the Z direction; x, Y, the directions are two directions perpendicular to each other on the horizontal plane, and the Z direction is the vertical direction; the first operating arm 7 and the second operating arm are used for suspending hydrate particles;
the visual reaction device is used for generating hydrate particles; the photographing/video recording system is used for acquiring the displacement of hydrate particles in the visual reaction device; the low-temperature constant-temperature control system is used for providing stable working temperature for the visual reaction device; the temperature acquisition instrument is used for measuring the working temperature of the visual reaction device in real time.
Example 2
An apparatus for measuring the microscopic adhesion between hydrate particles in a gas phase system as described in example 1, except that,
visual reaction unit includes control by temperature change circulation tank 11, circulation liquid import 8, circulation liquid export, operating element 10, double glazing window 9, and low temperature constant temperature control system is respectively through circulation liquid import 8, circulation liquid export through connection control by temperature change circulation tank 11, is provided with operating element 10 in the control by temperature change circulation tank 11, and operating element 10 side and the department of the corresponding position of system of shooing/recording are equipped with double glazing window 9.
The low-temperature constant-temperature tank 1 is respectively communicated with a circulating liquid inlet 8 and a circulating liquid outlet through a rubber pipeline 2, circulating liquid is input and output through the circulating liquid inlet 8 and the circulating liquid outlet, and a stable working temperature is provided for the operation unit 10 by utilizing the principle of circulating refrigeration; the photographing/video recording system acquires the displacement of hydrate particles in the operation unit 10 through the double-layer glass window 9; the ambient air is moist, and reaction temperature is lower, and visual reaction unit's window temperature is less than the room temperature, and the surface is covered with one deck water smoke easily, adopts double glazing window 9 can solve this water smoke problem.
The device also comprises a cyclopentane micro-supply device 13, and the cyclopentane micro-supply device 13 is communicated with the operation unit 10.
The operation unit 10 is provided with cyclopentane 28, and the cyclopentane 28 has strong volatility, so as to maintain the liquid amount in the operation unit 10 constant, a cyclopentane micro-supply device 13 is arranged, and the problem of liquid level reduction caused by volatilization of the cyclopentane 28 is solved by utilizing the siphon principle.
The length of the operation unit 10 is 3-4cm, the width of the operation unit 10 is 3-4cm, and the height of the operation unit 10 is 7-8 cm;
a deeper unit 10 facilitates a lower temperature of the gas in the unit 10 and a higher vapor concentration of cyclopentane 28 in the space near the bottom liquid level.
As shown in fig. 3, the first operation arm 7 includes a first metal arm 19, a first stainless steel thin tube 20 and a first glass fiber 21, one end of the first metal arm 19 is clamped on the first three-dimensional operation platform 3, the other end of the first metal arm 19 is welded to the first stainless steel thin tube 20, and the end of the first stainless steel thin tube 20 is connected to the first glass fiber 21. The first glass fiber 21 is used to suspend the hydrate particles.
The second operation arm comprises a second metal arm, a second stainless steel thin tube and second glass fibers, one end of the second metal arm is clamped on the second three-dimensional control platform, the other end of the second metal arm is welded with the second stainless steel thin tube, and the tail end of the second stainless steel thin tube is connected with the second glass fibers. The second glass fiber is used to suspend the hydrate particles.
The outer diameter of the first stainless steel tubule 20 is 0.5-0.8mm, and the stainless steel tubule in the outer diameter range is easy to be connected with the first glass fiber 21; the diameter of the first glass fiber 21 is 30-50um, the adhesion force among hydrate particles is small, and the deformation of the first glass fiber 21 with the diameter of 30-50um under the action of the adhesion force is easily obtained through the stereomicroscope 6. The outer diameter of the second stainless steel thin tube is 0.5-0.8mm, and the diameter of the second glass fiber is 50-100 um; the elastic coefficient of the second glass fiber in the diameter range is larger than that of the first glass fiber of 30-50um, so that only the first glass fiber of 30-50um in diameter is obviously deformed in the contact and separation process of hydrate particles, and the displacement of the hydrate particles can be conveniently measured.
The photographing/video recording system comprises a stereoscopic microscope 6 and a computer 4, the computer 4 is connected with the stereoscopic microscope 6 through a data line 5, and the stereoscopic microscope 6 obtains the displacement of hydrate particles in an operation unit 10 through a double-layer glass window 9; and measuring and analyzing the adhesive force by using Hooke's law according to the elastic coefficient of the glass fiber.
The device still includes visual cage 15, and first microcosmic operating system, second microcosmic operating system, visual reaction unit, stereomicroscope 6, temperature acquisition appearance, cyclopentane micro-supply device 13 all set up in visual cage 15, are equipped with operation window 16 on the visual cage 15. As shown in fig. 2.
The visual isolation hood 15 isolates the first microscopic operation system, the second microscopic operation system, the visual reaction device, the stereoscopic microscope 6, the temperature acquisition instrument and the cyclopentane micro-supply device 13 from the external environment, so that the air flow is reduced, and the volatilization rate of cyclopentane 28 is reduced; external dust and water vapor are effectively prevented from entering the operating environment, and the operating environment is kept relatively clean and dry; the visual cage 15 is provided with an operation window 16, so that the experiment operation is facilitated, and the operation window 16 is closed after the operation is finished.
The temperature acquisition instrument comprises a digital thermometer 14 and a probe, wherein the digital thermometer 14 is connected with the probe, the probe head of the probe extends into the operation unit 10, and the temperature of a gas phase system near the liquid level in the operation unit 10 is measured in real time.
The low-temperature constant-temperature control system is a low-temperature constant-temperature tank 1, and the low-temperature constant-temperature tank 1 is respectively connected with a circulating liquid inlet 8 and a circulating liquid outlet through a rubber pipeline 2.
The visual isolation cover 15 is made of transparent organic glass; the temperature control circulating tank 11 is made of stainless steel; the double-layer glass window 9 is made of high-transmittance colorless glass.
The visual isolation cover 15 is made of transparent organic glass, and the transparent organic glass can be used for conveniently observing the internal experimental state; the double glazing window 9 adopts high-transparency glass material, the operation is visual, the temperature control circulating groove 11 adopts stainless steel material, and the temperature in the control operation unit 10 and the strength of the device are convenient to control.
Example 3
The method for measuring the micro-adhesion force among hydrate particles in a gas phase system by using the device described in the embodiment 2 is shown in figure 4 and comprises the following steps:
A. determination of the modulus of elasticity of glass fibers
a. Clamping the first operating arm 7 on the first three-dimensional control platform 3, placing the small cone 22 on an object stage of the precision electronic balance 23, opening the precision electronic balance 23, and recording the reading m of the precision electronic balance 231；
b. Operating the first three-dimensional control platform 3 to enable the tail end of the first glass fiber 21 to be just contacted with the vertex of a small cone 22 on an object stage of a precision electronic balance 23;
c. the first Z operation platform 18 is operated to make the first operation arm 7 slowly descend 300-1And recording the reading m of the precision electronic balance 232；
d. Calculating the elastic coefficient of the glass fiber
e. Repeating the steps b-d30 times or more to obtain the average value of the elastic coefficient of the glass fiber
FIG. 5 shows 32 measurements of the modulus of elasticity of the glass fiber on the first operating arm 7, the average value
B. Producing hydrate particles in a gas phase system; the method comprises the following steps:
(1) injecting 20-30ml of cyclopentane solution (with the concentration of 96%) into the operation unit 10;
(2) adjusting the low-temperature constant-temperature tank 1 to enable the temperature of a gas phase system above the liquid level of cyclopentane 28 in the operation unit 10 to reach (-3) - (-2);
(3) a droplet 25 is made at the end of the first glass fiber 21 by the micro-syringe 24, the droplet 25 having a diameter d, 600um < d <700um, see in particular step ① in fig. 4;
(4) placing the droplets 25 in liquid nitrogen 26 for 20-30 seconds to produce first ice particles, using a liquid nitrogen tank 27 to contain the liquid nitrogen 26, see specifically step ② in FIG. 4;
(5) clamping the first operation arm 7 on the first three-dimensional operation platform 3, operating the first three-dimensional operation platform 3, and placing the first ice particles 3-5mm above the liquid level of the cyclopentane 28 in the operation unit 10, in particular, see step ③ in fig. 4;
(6) making a droplet in the middle of the second glass fiber, the droplet having a diameter d, 600um < d <700 um;
(7) putting the liquid drops into liquid nitrogen for 20-30s to manufacture second ice particles;
(8) clamping a second operation arm on a second three-dimensional operation platform, operating the second three-dimensional operation platform, and placing second ice particles at a position 3-5mm above the liquid level of cyclopentane 28 in an operation unit;
(9) and adjusting the low-temperature constant-temperature tank 1, increasing the temperature by 1 ℃ every 10min until the temperature of a gas phase system above the cyclopentane 28 solution reaches 0 ℃, keeping the temperature for 30min, and waiting for the first ice particles and the second ice particles to melt to generate first hydrate particles and second hydrate particles.
C. Measurement of the adhesion between hydrate particles in a gas phase System
(10) The low-temperature constant-temperature tank 1 is adjusted to make the temperature of the gas phase system in the operation unit 10 reach the experimental temperature T1，T1＝1℃；
(11) Starting a photographing/video recording system;
(12) operating the first three-dimensional control platform 3 and the second three-dimensional control platform to make the first hydrate particles and the second hydrate particles in the same vertical plane, that is, when the first hydrate particles and the second hydrate particles are vertically seen from the upper surface of the operation unit 10 to be overlapped, specifically referring to step ④ in fig. 4;
(13) operating the second three-dimensional manipulation platform to slowly move (9 ± 3um/s) the second hydrate particles to contact the first hydrate particles and apply a load △ P of 2uN to deform the first glass fibers 21 for 10s, see step ⑤ in fig. 4;
(14) operating the second three-dimensional control platform, and slowly moving (9 +/-3 um/s) the second hydrate particles to slowly separate the first hydrate particles from the second hydrate particles, specifically referring to step ⑥ in fig. 4, and referring to the step in fig. 4 after separation⑦, recording the end strain displacement △ x of the first glass fiber 21 just after the separation of the two hydrate particles by using a stereomicroscope 62The microscopic adhesion between hydrate particles is obtained by Hooke's law
FIG. 6 is a graph of an adhesion measurement taken of a sample after 30min of formation of hydrate particles in a gas phase system at 1 deg.C, using imagej software to measure △ x displacement of the end of the first glass fiber when the hydrate particles in FIG. 6 were separated2520.5um, therefore, adhesion
Claims (3)
1. A method for measuring the micro-adhesive force among hydrate particles in a gas phase system by adopting a device for measuring the micro-adhesive force among the hydrate particles in the gas phase system comprises a first micro-operation system, a second micro-operation system, a visual reaction device, a photographing/video recording system, a low-temperature constant-temperature control system and a temperature acquisition instrument;
the first microscopic operating system comprises a first three-dimensional control platform and a first operating arm clamped on the first three-dimensional control platform, and the first three-dimensional control platform comprises a first XY operating platform and a first Z operating platform;
the second micro operating system comprises a second three-dimensional control platform and a second operating arm clamped on the second three-dimensional control platform, and the second three-dimensional control platform comprises a second XY operating platform and a second Z operating platform;
the first XY operating platform and the second XY operating platform are used for accurately moving the hydrate particles in the X, Y direction; the first Z operation platform and the second Z operation platform are used for enabling hydrate particles to accurately move in the Z direction; the X, Y directions refer to two directions which are vertical to each other on a horizontal plane, and the Z direction refers to a vertical direction; the first operating arm and the second operating arm are used for suspending hydrate particles;
the visual reaction device is used for generating hydrate particles; the photographing/video recording system is used for acquiring the displacement of hydrate particles in the visual reaction device; the low-temperature constant-temperature control system is used for providing stable working temperature for the visual reaction device; the temperature acquisition instrument is used for measuring the working temperature of the visual reaction device in real time;
the visual reaction device comprises a temperature control circulating groove, a circulating liquid inlet, a circulating liquid outlet, an operating unit and a double-layer glass window, the low-temperature constant-temperature control system is respectively communicated with the temperature control circulating groove through the circulating liquid inlet and the circulating liquid outlet, the operating unit is arranged in the temperature control circulating groove, and the double-layer glass window is arranged on the side surface of the operating unit corresponding to the photographing/video recording system;
the device also comprises a cyclopentane micro-supply device which is communicated with the operation unit;
the first operation arm comprises a first metal arm, a first stainless steel thin tube and first glass fibers, one end of the first metal arm is clamped on the first three-dimensional control platform, the other end of the first metal arm is welded with the first stainless steel thin tube, and the tail end of the first stainless steel thin tube is connected with the first glass fibers;
the second operation arm comprises a second metal arm, a second stainless steel thin tube and second glass fibers, one end of the second metal arm is clamped on the second three-dimensional control platform, the other end of the second metal arm is welded with the second stainless steel thin tube, and the tail end of the second stainless steel thin tube is connected with the second glass fibers;
the outer diameter of the first stainless steel tubule is 0.5-0.8mm, the diameter of the first glass fiber is 30-50um, the outer diameter of the second stainless steel tubule is 0.5-0.8mm, and the diameter of the second glass fiber is 50-100 um;
the photographing/video recording system comprises a stereoscopic microscope and a computer, wherein the computer is connected with the stereoscopic microscope, and the stereoscopic microscope obtains the displacement of hydrate particles in the operation unit through the double-layer glass window; measuring and analyzing the adhesive force by using Hooke's law according to the elastic coefficient of the glass fiber;
the device also comprises a visual isolation hood, wherein the first microscopic operation system, the second microscopic operation system, the visual reaction device, the stereoscopic microscope, the temperature acquisition instrument and the cyclopentane micro-supply device are all arranged in the visual isolation hood, and an operation window is arranged on the visual isolation hood;
the temperature acquisition instrument comprises a digital thermometer and a probe, the digital thermometer is connected with the probe, a probe of the probe extends into the operation unit, and the temperature of a gas phase system near the liquid level in the operation unit is measured in real time;
the low-temperature constant-temperature control system is a low-temperature constant-temperature tank which is respectively connected with the circulating liquid inlet and the circulating liquid outlet through rubber pipelines;
the visual isolation cover is made of transparent organic glass; the temperature control circulating tank is made of stainless steel; the double-layer glass window is made of high-transmittance colorless glass; the method is characterized by comprising the following steps:
A. determination of the modulus of elasticity of glass fibers
B. Producing hydrate particles in a gas phase system; the method comprises the following steps:
(1) injecting 20-30ml of cyclopentane solution into the operation unit;
(2) adjusting the low-temperature constant-temperature tank to enable the temperature of a gas phase system above the liquid level of cyclopentane in the operation unit to reach (-3) - (2);
(3) producing a droplet at the end of the first glass fiber, the droplet having a diameter d, 600um < d <700 um;
(4) putting the liquid drops into liquid nitrogen for 20-30s to manufacture first ice particles;
(5) clamping the first operating arm on the first three-dimensional operating platform, operating the first three-dimensional operating platform, and placing first ice particles at a position 3-5mm above the liquid level of cyclopentane in an operating unit;
(6) creating a droplet in the middle of the second glass fiber, the droplet having a diameter d, 600um < d <700 um;
(7) putting the liquid drops into liquid nitrogen for 20-30s to manufacture second ice particles;
(8) clamping the second operating arm on the second three-dimensional operating platform, operating the second three-dimensional operating platform, and placing second ice particles at a position 3-5mm above the liquid level of cyclopentane in the operating unit;
(9) adjusting the low-temperature constant-temperature tank, increasing the temperature by 1 ℃ every 10min until the temperature of a gas phase system above the cyclopentane solution reaches 0 ℃, keeping the temperature for 30min, and waiting for the first ice particles and the second ice particles to melt to generate first hydrate particles and second hydrate particles;
C. measurement of the adhesion between hydrate particles in a gas phase System
(10) Adjusting the low-temperature constant-temperature tank to enable the temperature of a gas phase system in the operation unit to reach the experimental temperature T1，0℃<T1<7.7℃；
(11) Starting the photographing/recording system;
(12) operating the first three-dimensional control platform and the second three-dimensional control platform to enable the first hydrate particles and the second hydrate particles to be in the same vertical plane, namely, the first hydrate particles and the second hydrate particles are overlapped when the upper surface of the operation unit vertically downwards looks;
(13) operating the second three-dimensional control platform, slowly moving the second hydrate particles to contact the first hydrate particles, and applying a load △ P, wherein 2uN is more than △ P and less than 8uN, so that the first glass fibers are deformed and kept for 10 s;
(14) operating the second three-dimensional control platform, slowly moving the second hydrate particles to slowly separate the first hydrate particles from the second hydrate particles, and recording the terminal deformation displacement delta x of the first glass fiber when the two hydrate particles are just separated by using the stereoscopic microscope2The microscopic adhesion between hydrate particles is obtained by Hooke's law
2. The method for measuring the micro-adhesion force between hydrate particles in a gas phase system by using the device for measuring the micro-adhesion force between hydrate particles in a gas phase system according to claim 1, wherein the length of the operation unit is 3-4cm, the width of the operation unit is 3-4cm, and the height of the operation unit is 7-8 cm.
3. The method for measuring the micro-adhesion force between hydrate particles in a gas phase system by using the device for measuring the micro-adhesion force between hydrate particles in a gas phase system according to claim 1, wherein the step A comprises the steps of:
a. clamping a first operating arm on a first three-dimensional control platform, placing a small cone on an object stage of a precision electronic balance, opening the precision electronic balance, and recording the reading m of the precision electronic balance1；
b. Operating the first three-dimensional control platform to enable the tail end of the first glass fiber to be just contacted with the vertex of a small cone on an objective table of the precision electronic balance;
c. operating the first Z operating platform to make the first operating arm slowly descend for 300-1And recording the reading m of the precision electronic balance2；
d. Calculating the elastic coefficient of the glass fiber
e. Repeating the steps b-d30 times or more to obtain the average value of the elastic coefficient of the glass fiber
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| CN109323986B (en) * | 2018-11-30 | 2020-06-26 | 中国地质大学（武汉） | Device and method for testing adhesion force between gas hydrate and mineral particles |
| CN109883946B (en) * | 2019-01-25 | 2021-05-14 | 华南理工大学 | High-pressure-resistant microscopic observation constant-temperature table with cantilever operation |
| CN110108626A (en) * | 2019-05-11 | 2019-08-09 | 金华职业技术学院 | A kind of adherency force test device based on micro- tweezer |
| CN110346285B (en) * | 2019-07-22 | 2021-09-14 | 中国石油大学(华东) | Mechanical property detection device and force detection system |
| CN112098320B (en) * | 2020-09-15 | 2022-08-26 | 常州大学 | Testing device for adhesive force between gas hydrate particles and wax crystal particles |
| CN112691610A (en) * | 2020-12-25 | 2021-04-23 | 中国石油大学(华东) | High-pressure visual microscopic acting force testing device |
| CN113029727A (en) * | 2021-04-26 | 2021-06-25 | 常州大学 | Adhesion testing device capable of forming regular spherical hydrate particles |
| CN114609337B (en) * | 2022-03-11 | 2023-03-10 | 中国石油大学(华东) | Microscopic and macroscopic evaluation method of double-effect hydrate inhibitor |
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