CN109883946B - High-pressure-resistant microscopic observation constant-temperature table with cantilever operation - Google Patents
High-pressure-resistant microscopic observation constant-temperature table with cantilever operation Download PDFInfo
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- CN109883946B CN109883946B CN201910071095.9A CN201910071095A CN109883946B CN 109883946 B CN109883946 B CN 109883946B CN 201910071095 A CN201910071095 A CN 201910071095A CN 109883946 B CN109883946 B CN 109883946B
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Abstract
The invention discloses a high-pressure-resistant microscopic observation constant-temperature table with cantilever operation. The constant temperature table comprises a detachable left side wall surface, a visible window, fins, a fixed right side wall surface, fixed front and rear side walls, a fixed top wall surface and a temperature control medium channel; the detachable left side wall surface, the fixed front side wall, the fixed rear side wall and the fixed top wall surface form a closed space, a sunken cooling table is arranged below the space, and fins are arranged on the sunken wall surface; a visible window is arranged on the fixed top wall surface; a fixed baffle is arranged on the detachable left side wall surface; the detachable left side wall surface is provided with a hole groove, and an operable cantilever penetrates through the hole groove. The constant temperature platform can directly observe the nucleation and growth process of the gas hydrate particles in a microscopic way under the high pressure condition, measure the adhesive force among the gas hydrate particles and evaluate the performance of the hydrate inhibitor, and has the advantages of simple device and convenient operation.
Description
Technical Field
The invention relates to the flow safety of an oil and gas pipeline and the growth dynamics of a gas hydrate, in particular to a high-pressure-resistant microscopic observation constant temperature platform with cantilever operation.
Technical Field
The gas hydrate is mainly an ice-like crystal structure formed by a guest molecule (such as methane, ethane, propane, carbon dioxide, hydrogen sulfide and the like) and a water molecule through van der Waals force under certain environmental conditions. During the process of exploiting hydrates and transporting oil and gas pipelines, water and natural gas in the pipelines are easy to combine together to form hydrate particles due to the low-temperature and high-pressure environment in the pipelines, and further aggregate and agglomerate to block the pipelines, so that the exploitation efficiency is reduced and the production is stopped, which troubles the production and transportation of oil and gas for a long time.
The adhesion of hydrate particles is an important index influencing the aggregation tendency of hydrates, and in order to solve the problem that the oil and gas pipeline hydrates are agglomerated to block the pipeline, scholars develop a set of high-pressure-resistant micromanipulation devices and investigate the influence of various factors on the adhesion of the hydrate particles. However, the device is complicated, and the operating arm and the driving system are in a high-pressure environment, which requires pressure resistance and explosion resistance. The operating arm and the driving system of the device are in a normal pressure environment, the pressure resistance requirement of the equipment is greatly reduced, and the equipment has small volume and low cost. In addition, no report is found in microscopic observation experiments of the generation, growth and aggregation of gas hydrate crystals under pressure.
Based on the problems, the invention provides the high-pressure-resistant microscopic observation constant-temperature table with the cantilever operation, which has the advantages of small volume, simple device, convenient operation and low cost, can directly measure the adhesive force among gas hydrate particles under the high-pressure condition, evaluate the performance of an additive, and perform microscopic observation to study the generation, growth and aggregation of pressurized gas hydrate crystals, thereby filling the blank of the study on the aspect.
Disclosure of Invention
The invention aims to provide a high-pressure-resistant microscopic observation constant-temperature table with cantilever operation, which is used for microscopically observing the growth and nucleation process of gas hydrate and measuring the adhesive force among pressurized gas hydrate particles.
The technical scheme of the invention is as follows:
a high-pressure-resistant microscopic observation constant-temperature table with cantilever operation comprises a detachable left side wall surface, a visible window, fins, a fixed right side wall surface, fixed front and rear side walls, a fixed top wall surface and a temperature control medium channel; the detachable left side wall surface, the fixed front side wall, the fixed rear side wall and the fixed top wall surface form a closed space, a sunken cooling table is arranged below the space, and fins are arranged on the sunken wall surface; a visible window is arranged on the fixed top wall surface; a fixed baffle is arranged on the detachable left side wall surface; the detachable left side wall surface is provided with a hole groove, an operable cantilever penetrates through the hole groove, the operable cantilever penetrates through the fixed baffle and extends into the closed space, the flexible material covers the baffle and the left wall, and the detachable left side wall surface is provided with a temperature sensor; a fixed cantilever, an air inlet channel and a pressure sensor are arranged on the fixed right side wall surface; the inner side of the cooling table is provided with fins for enhancing the uniform distribution of heat transfer.
Furthermore, a temperature control medium channel is arranged around the outer ring of the cooling table, and a pipeline is connected outside the temperature control medium channel; the temperature control medium channel is of an annular structure.
Further, the cold stage is made of stainless steel, and the centers of the upper surface and the lower surface of the cold stage are respectively provided with a visual window (sapphire, quartz glass and polycarbonate).
Furthermore, operation cantilevers are installed on the left wall surface and the right wall surface above the cooling table, wherein the left wall surface is a detachable wall surface and is provided with a movable operation cantilever, and the right wall surface is provided with a fixed cantilever; the operable cantilever end is inserted with glass fiber, and the connection mode is that the operable cantilever end is inserted.
Furthermore, a hole groove is formed in the left side wall surface above the cold table, an operable cantilever with a baffle passes through the hole groove, the baffle is arranged on the left side upper wall surface of the cold table and is tightly attached to the left side upper wall surface of the cold table, and the cantilever can move left and right along the hole groove.
Further, the flexible material is a rubber film, a polyethylene film or a silicon film, and when air enters, the flexible material can be tightly attached to the baffle and the left side wall surface, so that air leakage of the device is prevented.
Further, the temperature control medium in the temperature control medium channel is ethylene glycol, alcohol or silicone oil.
Compared with the prior art, the invention has the advantages that:
the device is simple, convenient to operate and low in cost, and can be used for directly observing the morphology and dynamic changes of gas hydrate particles.
Because THE invention can directly measure THE adhesive force among THE gas hydrate particles under high pressure, compared with THE traditional measurement of THE adhesive force of CP or THE hydrate particles formed under normal pressure, THE conclusion is more reliable.
The method can measure the adhesive force of the pressurized gas hydrate particles, calculate the growth rate and the nucleation time of the hydrate particles by utilizing statistics, and evaluate the performance of the low-dosage hydrate inhibitor.
Drawings
FIG. 1 is a cross-sectional view of a high pressure resistant microscopic observation thermostatic table with cantilever operation provided by the invention.
The various components in the figure are as follows: 1-operable cantilever, 2-temperature sensor, 3-detachable left side wall surface, 4-baffle, 5-flexible material, 6-visual window, 7-fin, 8-fixed right side wall surface, 9-air inlet channel, 10-fixed cantilever, 11-pressure sensor and 12-temperature control medium channel.
Fig. 2 is a schematic view of a removable left side wall configuration.
Fig. 3 hydrate particle "contact-offset-movement-separation" image.
Detailed Description
The present invention will be described in further detail with reference to specific examples
As shown in fig. 1 and 2, a high pressure-resistant microscopic observation thermostatic station with cantilever operation comprises a detachable left side wall surface 3, a visible window 6, fins 7, a fixed right side wall surface 8, fixed front and rear side walls, a fixed top wall surface and a temperature control medium channel 12; the detachable left side wall surface 3, the fixed front and rear side walls and the fixed top wall surface form a closed space, a sunken cooling platform is arranged below the space, and fins 7 are arranged on the sunken wall surface; a visible window 6 is arranged on the fixed top wall surface; a fixed baffle 4 is arranged on the detachable left side wall surface 3; the detachable left side wall surface 3 is provided with a hole groove, an operable cantilever 1 penetrates through the hole groove, the operable cantilever 1 penetrates through a fixed baffle 4 and extends into the closed space, the flexible material 5 covers the baffle 4 and the left wall 3, and the detachable left side wall surface 3 is provided with a temperature sensor 2; the fixed right side wall surface 8 is provided with a fixed cantilever 10, an air inlet channel 9 and a pressure sensor 11; the inner side of the cooling platform is provided with fins 7 for enhancing the uniform distribution of heat transfer. A temperature control medium channel 12 is arranged around the outside of the cooling platform, and a pipeline is connected outside the temperature control medium channel 12; the temperature-controlled shut-off channel 12 is of an annular configuration. The material of the cold stage is selected from stainless steel. The operable cantilever 1 is inserted with glass fiber at the end, and the connection mode is that the end of the cantilever is inserted. The wall surface of the left side above the cold table is provided with a hole groove, an operable cantilever with a baffle plate 4 passes through the hole groove, the baffle plate 4 is arranged on the wall surface of the left side above the cold table and is tightly attached to the wall surface, and the cantilever moves left and right along the hole groove. The flexible material 5 is a rubber film, a polyethylene film or a silicon film. The temperature control medium in the temperature control medium channel is ethylene glycol, alcohol or silicone oil.
Example 1
1. The operable cantilever 1 is inserted into the hole slot of the detachable left side wall 3 and a small drop (300 μm-500 μm in diameter) of deionized water is injected with a micro-syringe onto the ends of the two cantilever glass fibers.
2. The gap between the cantilever baffle 4 and the detachable left side wall surface 3 is sealed by a flexible material 5, and the detachable left side wall surface 3 is installed on the cold stage. The detachable left side wall 3 is mounted on the cold plate by inserting the operable boom 1 into the hole of the detachable left side wall 3 and sealing the gap between the boom baffle 4 and the detachable left side wall 3 with the flexible material 5.
3. Introducing CH of 6MPa4And opening the temperature and pressure sensor to set the temperature to 30 ℃ and maintain the temperature for one hour to eliminate the memory effect, and opening the camera to shoot and record the growth of the hydrate particles.
4. Reducing the temperature to 2 ℃ required by the experiment at a certain rate, and recording the temperature reduction time t1Maintaining the temperature until hydrate crystal nucleus appears on the water drop, and recording the time t2And recording the growth process of the hydrate, wherein the nucleation time t is t1-t2，
5. When the complete conversion of the droplets into hydrate particles was recorded at this timeTime t3(solid spherical solid particles, the growth end point is the surface appearance and luster of the solid spherical solid particles, and the growth time of the hydrate is T ═ T-3-t2The growth rate of hydrate particles is V ═ pi D3The ratio of D to D is the hydrate particle diameter, which is generally from 400 to 700. mu.m.
6. The above operation was repeated 20 times, and the hydrate nucleation time and growth rate were calculated by a statistical method.
Example 2
1. A small drop (300 μm to 500 μm in diameter) of 0.5 wt% concentration of the anti-agglomerant polyvinyl alcohol (PVA) was injected with a micro-syringe onto the end of two cantilever glass fibers.
2. The operational cantilever 1 is inserted into the hole groove of the detachable left side wall surface 3, and the gap between the cantilever baffle and the detachable left side wall surface 3 is sealed by flexible materials, and the left side wall surface is installed on the cold stage.
3. The temperature of the cooling table is reduced to-5 ℃, and 74.3 percent CH with the pressure of 5MPa is introduced4+25.7％C2H6。
4. Once hydrate nucleation was observed, the temperature was raised to 1 ℃ and annealed for 15 h.
5. Keeping the hydrate particles a and B at rest for 10s, allowing the center of the hydrate particles to reach equilibrium (as shown in fig. 3A), moving the operable cantilever 1 to make the two particles contact with each other, and applying a certain pressure to keep for 10s (as shown in fig. 3B), then slowly moving the particles a, wherein the two particles move under the action of the adhesive force and have adhesive deviation (as shown in fig. 3C) due to the adhesive force between the particles, and the particles B return to the original equilibrium position (as shown in fig. 3D) due to the elastic action of the glass fiber.
6. The above operation was repeated 40 times, and the hydrate particle adhesion-separation process was photographed and recorded with a microscope.
7. And (4) measuring and calculating the adhesion force among the hydrate particles according to Hooke's law.
8. When the calculated adhesion is less than a standard value of 40mN/m (the adhesion value of the hydrate particles tested by researchers without adding the low-dosage hydrate inhibitor under the same conditions), the adhesion of the hydrate particles can be reduced by the anti-agglomerant, and the smaller the value, the better the viscosity reduction effect of the low-dosage hydrate inhibitor is.
The above examples are given for the purpose of illustrating the invention in a clear and clear manner, and it will be apparent to those skilled in the art that various other modifications and variations can be made in the above examples without departing from the scope of the invention.
Medium
Claims (7)
1. A high-pressure-resistant microscopic observation constant-temperature table with cantilever operation is characterized by comprising a detachable left side wall surface (3), a visible window (6), fins (7), a fixed right side wall surface (8), fixed front and rear side walls, a fixed top wall surface and a temperature control medium channel (12); the detachable left side wall surface (3), the fixed front side wall, the fixed rear side wall, the fixed top wall surface and the fixed right side wall surface form a closed space, a sunken cooling table is arranged below the space, and fins (7) are arranged on the sunken cooling table; a visible window (6) is arranged on the fixed top wall surface; a fixed baffle (4) is arranged on the detachable left side wall surface (3); a hole groove is formed in the detachable left side wall surface (3), an operable cantilever (1) penetrates through the hole groove, the operable cantilever (1) penetrates through the fixed baffle (4) and extends into the closed space, the flexible material (5) covers the baffle (4) and the detachable left side wall surface (3), and a temperature sensor (2) is arranged on the detachable left side wall surface (3); a fixed cantilever (10), an air inlet channel (9) and a pressure sensor (11) are arranged on the fixed right side wall surface (8); the inner side of the cooling platform is provided with fins (7) for strengthening the uniform distribution of heat transfer.
2. The high-pressure-resistant microscopic observation constant-temperature table with cantilever operation according to claim 1, wherein a temperature-control medium channel (12) is arranged around the outside of the cold table, and a pipeline is connected outside the temperature-control medium channel (12); the temperature control medium channel (12) is of an annular structure.
3. The high pressure resistant microscopic observation constant temperature stage with cantilever operation of claim 1, wherein the material of the cold stage is selected from stainless steel.
4. The high-pressure-resistant microscopic observation thermostatic table with cantilever operation according to claim 1, wherein the operable cantilever (1) has a terminal inserted with glass fiber, and the connection mode is that the terminal is inserted.
5. The high pressure resistant microscopic observation thermostatic table with cantilever operation according to claim 1, wherein a hole slot is opened on the left side wall surface above the cold table, the operable cantilever with the baffle (4) passes through the hole slot, the baffle (4) is arranged on the left side wall surface above the cold table and is tightly attached to the left side wall surface, and the cantilever moves left and right along the hole slot.
6. The high-pressure-resistant microscopic observation constant-temperature table with cantilever operation according to claim 1, wherein the flexible material (5) is a rubber film, a polyethylene film or a silicone film.
7. The high-pressure-resistant microscopic observation constant-temperature table with cantilever operation according to claim 2, wherein the temperature-control medium in the temperature-control medium channel is ethylene glycol, alcohol or silicone oil.
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| JPH10206312A (en) * | 1997-01-27 | 1998-08-07 | Olympus Optical Co Ltd | Micro body adhesion force measuring device |
| CN206208884U (en) * | 2016-10-31 | 2017-05-31 | 华南理工大学 | A kind of device of accurate surveying gas hydrate induction time |
| CN107024428A (en) * | 2017-04-24 | 2017-08-08 | 中国石油大学(华东) | A kind of experimental provision and its method of work for visualizing hydrate wall adhesion mechanics characteristic |
| CN108535180A (en) * | 2018-04-04 | 2018-09-14 | 中国石油大学(华东) | A kind of device and method for measuring microcosmic adhesion strength between hydrate particle in gas phase system |
| CN108519384A (en) * | 2018-04-17 | 2018-09-11 | 中国石油大学(华东) | A kind of normal pressure visualization device and method generated in porous media for simulating hydrate with decomposition |
| CN108827839A (en) * | 2018-08-28 | 2018-11-16 | 广州海洋地质调查局 | Micro- force test device and its test method between a kind of natural gas hydrate stratum particle |
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