CN111239132A - Visual high-pressure microfluidic hydrate simulation experiment device and application thereof - Google Patents

Visual high-pressure microfluidic hydrate simulation experiment device and application thereof Download PDF

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CN111239132A
CN111239132A CN202010062969.7A CN202010062969A CN111239132A CN 111239132 A CN111239132 A CN 111239132A CN 202010062969 A CN202010062969 A CN 202010062969A CN 111239132 A CN111239132 A CN 111239132A
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CN111239132B (en
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徐加放
王博闻
王晓璞
赵欣
曹杰
丁廷稷
张雪
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China University of Petroleum East China
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    • GPHYSICS
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Abstract

The invention discloses a visual high-pressure microfluidic hydrate simulation experiment device and application thereof, which comprises a micro-fluid injection and pressure control unit, a pressure-resistant microfluidic hydrate reaction unit, a temperature control unit, a generated gas processing unit and a real-time display unit, wherein all the units are connected through pipelines or data lines and controlled through corresponding valves or switches; the real-time clear observation can be carried out on the microscopic process of the hydrate reaction; and can complete various types of experiments aiming at the reaction characteristics of the gas hydrate in the micropores/throats, and has good experimental operability and comprehensiveness.

Description

Visual high-pressure microfluidic hydrate simulation experiment device and application thereof
Technical Field
The invention belongs to the technical research field of hydrates, and particularly relates to a visual high-pressure microfluidic hydrate simulation experiment device and application thereof.
Background
The gas hydrate is a non-stoichiometric cage-shaped solid crystal, which is an envelope-shaped crystal formed by interaction of one or more gases or volatile liquid and water in a high-pressure and low-temperature environment. Wherein, the natural gas hydrate is a crystal compound composed of water molecules and hydrocarbon gas molecules, belongs to a clean energy, and generates water and CO after being combusted in the air2And the pollution to the environment is small. The natural gas hydrate is widely distributed, and is mostly distributed in deep water sediments and land permafrost. At present, the natural gas hydrate reserves which have been ascertained worldwide are about 2.84 times as much as the global non-renewable energy sources. Compared with the traditional energy sources (coal and petroleum), the natural gas hydrate has the characteristics of cleanness, abundant reserves, high energy density and the like, and has extremely high resource value. Therefore, the natural gas hydrate has extremely high research value and becomes a hot spot for the research of scholars at home and abroad.
In the experimental study of hydrates, phase studies, inhibitor evaluations, and optimization of production methods have been focused on in many cases. In the research on the aspects, a large-size reaction kettle or a closed sand filling cylinder is mostly adopted for experimental exploration, the micropore form of a porous medium is difficult to accurately simulate in the experimental process, and the micro-reaction process of the hydrate cannot be intuitively observed in real time.
Microfluidic technology is an emerging technology for precisely manipulating micro-fluid. Because the method has short analysis time, high sensitivity and small error compared with the traditional experimental means, the microfluidics has been developed into a brand-new research field crossed with the disciplines of biology, chemistry, medicine, fluid, electronics, materials, machinery and the like. The advantages of the microfluidic chip make it suitable for the research on the behavior of hydrate phase in the porous medium of the simulated stratum: (1) the transparent material of the microfluidic chip eliminates the black box effect of the traditional method and realizes the real-time observation of the inside of the system; (2) the micron-scale pore etching technology can accurately copy a complex hydrate stratum micropore structure; (3) the micro-fluid regulation technology can accurately control the pressure and the flow rate of the fluid in the chip so as to better quantitatively research the phase reaction of the hydrate in the micropores.
Chinese patent document CN106969957A discloses a multifunctional gas hydrate experimental system, which comprises a reaction kettle unit, a temperature control unit, a pressure control unit, a data acquisition unit and a monitoring unit. The reaction kettle unit comprises a high-pressure visible reaction kettle of core equipment; the temperature control unit controls the temperature in the reaction kettle by a constant-temperature water bath; the pressure control unit is used for introducing/discharging gas or solution into/from the reaction kettle and controlling the pressure in the reaction kettle; the data acquisition unit acquires and analyzes the data of the units; the monitoring unit monitors the experiment by a plurality of different testing means such as gas chromatography, raman spectroscopy and the like. However, the high-pressure visible reaction kettle disclosed in the patent cannot simulate the porous medium environment under the formation condition, and the actual reaction condition of the hydrate in the micropores is difficult to study. And the multifunctional gas hydrate experimental system device and the pipeline valve are very complicated and are relatively complex to operate.
Chinese patent document CN108519384A discloses an atmospheric pressure visualization device and method for simulating generation and decomposition of hydrate in porous medium, comprising a low temperature constant temperature control system, an atmospheric pressure visualization reaction device, a three-dimensional precision moving platform, a temperature acquisition instrument and a real-time display system; the normal-pressure visual reaction device comprises a temperature control circulation box, two reaction tanks which are embedded from top to bottom, a circulation liquid inlet and a circulation liquid outlet. The two reaction tanks can respectively observe the generation and decomposition processes of the hydrate in the sandstone porous medium and the generation and decomposition processes of the hydrate in the throat of the microscopic etching model. However, the normal pressure visualization device for simulating generation and decomposition of the hydrate in the porous medium described in the patent uses cyclopentane to perform experiments under atmospheric pressure conditions, and the natural gas hydrate is mainly generated and stored from methane gas hydrate under low temperature and high pressure conditions, so the device cannot simulate the reaction environment and the reaction process of the gas hydrate under real formation conditions; and the optical performance of the body type microscope used by the device is limited, and the phase interface in the hydrate reaction process is difficult to clearly represent.
Disclosure of Invention
The invention provides a visual high-pressure micro-fluidic hydrate simulation experiment device aiming at the defects of the prior art and aiming at exploring the micro reaction process of a gas hydrate in a micropore.
Compared with the existing experimental device, the invention has the beneficial effects that:
(1) the invention can accurately simulate the real low-temperature high-pressure environment of the natural gas hydrate in the stratum porous medium by applying the microfluidic technology;
(2) the invention can accurately control the fluid pressure and flow rate in the chip by applying the micro-fluid regulation and control technology so as to better quantitatively research the influence factors of the hydrate phase reaction in the formation micropores;
(3) the invention can clearly observe the reaction microscopic process of the hydrate in the micropore of the porous medium in real time;
(4) the invention can complete various experiments aiming at the reaction characteristics of the gas hydrate in the micropores/throats, such as simulation of generation and decomposition of the hydrate in the formation micropores, evaluation of the effect of a hydrate inhibitor solution, replacement exploitation of the natural gas hydrate and the like, has good experimental operability and comprehensiveness, and can provide theoretical support and optimization basis for the research of the micro reaction process of the gas hydrate in a porous medium. .
Drawings
Fig. 1 is a schematic diagram of a visual high-pressure microfluidic hydrate simulation experiment device according to the invention.
A. The system comprises a micro-fluid injection and pressure control unit, a pressure-resistant micro-fluidic hydrate reaction unit, a temperature control unit, a generated gas processing unit, a real-time display unit, a micro-fluid injection and pressure control unit, a pressure-resistant micro-fluidic hydrate reaction unit, a temperature control unit, a micro-fluid injection and pressure-resistant micro-fluidic hydrate reaction unit, a micro;
1. the device comprises a precision high-pressure injection pump, 2, a pressure-resistant injector, 3, 4, 7, 15, 16, a gas-liquid valve, 5, 6, a gas cylinder, 8, a digital pressure gauge, 9, a micro-cooling pump, 10, a temperature control table, 11, a pressure-resistant micro-fluidic glass chip, 12, an optical phase difference microscope, 13, a computer, 14 and an emptying valve.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the accompanying drawings and the detailed description.
The invention provides a visual high-pressure microfluidic hydrate simulation experiment device which comprises a micro-fluid injection and pressure control unit A, a pressure-resistant microfluidic hydrate reaction unit B, a temperature control unit C, a generated gas processing unit D and a real-time display unit E, wherein the micro-fluid injection and pressure control unit A is connected with the pressure-resistant microfluidic hydrate reaction unit B; the micro-fluid injection and pressure control unit A quantitatively injects gas or solution to the pressure-resistant micro-fluidic chip where the hydrate is located and accurately adjusts the pressure in the chip where the hydrate reacts; the core of the pressure-resistant microfluidic hydrate reaction unit B mainly comprises a plurality of pressure-resistant microfluidic glass chips 12; the temperature control unit C can accurately control the temperature of the chip where the hydrate reaction is positioned; the generated gas processing unit D can dry products in the hydrate reaction process, measure the flow of gas products and collect reaction gas; the real-time display unit E can observe the reaction process of the hydrate in the micropores of the pressure-resistant glass chip in real time. The units are connected through pipelines or data lines and are controlled through corresponding valves or switches.
The micro-fluid injection and pressure control unit A comprises a precise high-pressure injection pump 1, a pressure-resistant injector 2, a plurality of small gas cylinders 5 and 6 with regulating valves, a digital pressure gauge 8, a plurality of regulating valves 3, 4, 7, 15, 16 and 14 and pipelines, wherein 3, 4, 7, 15 and 16 are gas-liquid valves, and 14 is an emptying valve; the precise high-pressure injection pump 1 can quantitatively inject gas or solution into the pressure-resistant microfluidic hydrate reaction unit B at a constant flow rate by controlling the pressure-resistant injector 2; the gas bottles 5 and 6 supply gas into the pressure-resistant injector 2; the gas channel is closed, after the pressure-resistant injector 2 pumps liquid, the liquid can be injected into the pressure-resistant microfluidic hydrate reaction unit B through the precision high-pressure injection pump 1, and the pressure control of the hydrate reaction is realized by adjusting the liquid injection speed and corresponding valves; the digital pressure gauge 8 is positioned on a pipeline directly connected with the pressure-resistant micro-fluidic glass chip 11 and can display the pressure in the hydrate reaction process in real time.
The pressure-resistant microfluidic hydrate reaction unit B comprises a plurality of pressure-resistant microfluidic glass chips 11 etched with micron-sized pore channels to simulate hydrate formation micropores; injecting deionized water or solution into micropores etched by the pressure-resistant micro-fluidic glass chip 11 through a pipeline, injecting hydrate to generate corresponding gas for reaction, and adjusting the temperature control unit C and the micro-fluid injection and pressure control unit A to enable the interior of the pressure-resistant micro-fluidic glass chip 11 to reach the temperature and pressure conditions required by hydrate reaction; the pressure-resistant micro-fluidic glass chip 11 is fixed on the temperature control table 10 through a clamp and is connected with the micro-fluid injection and pressure control unit A through a stainless steel pipeline and a joint.
The temperature control unit C comprises a temperature control table 10 and a micro cooling pump 9, wherein the temperature control table 10 is connected with the micro cooling pump 9 through a heat preservation pipeline; the temperature and flow rate of the circulating cooling liquid can be set by the micro cooling pump 9; the temperature control table 10 heats up, cools down the circulating cooling liquid pumped by the micro cooling pump through the semiconductor heating device inside the temperature control table, and can display the surface temperature of the circulating cooling liquid in real time; the temperature control platform 10 is arranged on an object stage of an optical phase difference microscope 12, and a glass light transmission hole is formed in the middle of the temperature control platform and can enable a light source of the optical phase difference microscope to transmit; the pressure-resistant micro-fluidic glass chip 11 is placed in a constant-temperature area of the temperature control table 10; because the pressure-resistant micro-fluidic glass chip 11 is very thin (3mm), is completely attached to the temperature control table, and has a good heat transfer effect, the surface temperature of the temperature control table 10 can be considered as the temperature of the pressure-resistant micro-fluidic glass chip 9.
The generated gas processing unit D comprises a drying device 17, a gas micro-flow meter 18 and a gas collecting device 19; the drying device 17 contains an excessive calcium chloride drying agent; the gas-liquid mixture generated in the hydrate reaction process firstly passes through a gas micro-flowmeter 18 after being dried by a drying device 17; the gas micro-flow meter 18 can measure the real-time flow and the accumulated flow in the reaction process of the hydrate; the gas collecting device 19 can collect the gas generated by the hydrate reaction, and if necessary, the gas can be sent to a detector to analyze the collected gas components.
The real-time display unit E comprises an optical phase difference microscope 12 and a computer 13; the optical phase difference microscope 12 is provided with a plurality of objective lenses for phase difference observation, the maximum magnification can reach 1000 times, the maximum resolution can reach 0.27 mu m, the reaction behavior of the hydrate in the micropore can be clearly observed, and the phase interface of the hydrate-gas-liquid three phase can be accurately displayed; the optical phase difference microscope 12 is connected with a computer through a data line, and the microscopic morphology of the hydrate in the pressure-resistant micro-fluidic glass chip can be obtained in real time through image processing software on the computer.
The visual high-pressure microfluidic hydrate simulation experiment device can complete various different types of hydrate reaction experiments.
Specifically, the visual high-pressure microfluidic hydrate simulation experiment device is used for simulating the generation and decomposition of the hydrate in the formation micropores, and CH in a deionized water system is used4The hydrate is generated and decomposed as an example, and the experimental process is as follows by combining the figure 1:
the pressure-resistant syringe 2 is filled with deionized water and the gas cylinder 5 is filled with CH4All valves are closed by default in the initial state;
step 1: opening gas- liquid valves 3 and 7 and an emptying valve 14, operating a precise high-pressure injection pump 1 to enable a pressure-resistant injector 2 to start injecting deionized water, and enabling micropores etched by a pressure-resistant micro-fluidic glass chip 11 to be completely filled with deionized water;
step 2: after the step 1 is finished, the precise high-pressure injection pump 1 is operated to stop the injection of the pressure-resistant injector 2, the gas-liquid valve 3 and the vent valve 14 are closed, the gas-liquid valve 4 and the gas bottle 5 are opened, and the quantitative injection of CH into the pressure-resistant micro-fluidic glass chip 11 is started4After a proper amount of gas is injected, the gas-liquid valve 4 and the gas bottle 5 are closed;
and step 3: after the step 2 is finished, operating the micro cooling pump 9 to enable the temperature control table 10 to reach the temperature required by the generation of the hydrate and keeping the temperature unchanged;
and 4, step 4: after the step 3 is finished, opening gas- liquid valves 3 and 15, operating the precise high-pressure injection pump 1 to enable the pressure-resistant injector 2 to simultaneously inject deionized water to two ends of the pressure-resistant microfluidic glass chip 11 to increase pressure, observing a digital pressure gauge 8, controlling the precise high-pressure injection pump 1 to enable the pressure-resistant injector 2 to stop injecting when the pressure reaches the pressure required by hydrate generation, closing the gas- liquid valves 3, 7 and 15, and displaying the pressure in the micropore of the pressure-resistant microfluidic glass chip 11 by the pressure gauge;
and 5: after the step 4 is finished, observing the generation process of the hydrate in real time through image processing software carried by an optical phase difference microscope 12 and a computer 13, and acquiring pictures and videos of the hydrate in the micropores for subsequent analysis until the hydrate form is not changed and the value of a pressure gauge is stable;
step 6: and (5) after the step (5) is finished, opening the vent valve (14), observing the decomposition process of the hydrate, opening the gas-liquid valves (3, 7 and 15) after the hydrate is completely decomposed, injecting deionized water through the pressure-resistant injector (2) to clean the pipeline and the pressure-resistant microfluidic glass chip (11), and properly collecting experimental waste gas and waste liquid.
Example 2:
the difference from example 1 is: the visual high-pressure microfluidic hydrate simulation experiment device is used for the effect evaluation experiment of the hydrate inhibitor solution, and CH is used4The induction times of the gas in 5 wt% and 10 wt% NaCl solutions to form hydrates are compared as an example, and the experimental process is as follows with reference to FIG. 1:
the gas cylinder 5 is filled with CH4All valves are closed by default in the initial state;
step 1: opening gas- liquid valves 3 and 7 and an emptying valve 14, operating a precise high-pressure injection pump 1 to enable a pressure-resistant injector 2 to start injecting 5 wt% NaCl solution, and enabling micropores etched by a pressure-resistant micro-fluidic glass chip 11 to be completely filled with 5 wt% NaCl solution;
step 2: after the step 1 is finished, continuously injecting 5 wt% NaCl solution until the solution in the pressure-resistant injector 2 is exhausted, closing the gas-liquid valve 7 and the vent valve 14, opening the gas-liquid valve 4 and the gas bottle 5, and controlling the precision high-pressure injection pump 1 to enable the pressure-resistant injector 2 to suck proper amount of CH4And recording the suction volume V and the reading P of the pressure gauge on the gas cylinder1
And step 3: after the step 2 is finished, closing the gas-liquid valve 4 and the gas bottle 5, opening the gas-liquid valve 7, and controlling the precision high-pressure injection pump 1 to enable the precision high-pressure injection pump to be startedPressure resistant Syringe 2 injects all CH aspirated in step 24Then the gas-liquid valve 3 is closed;
and 4, step 4: after the step 3 is finished, the micro cooling pump 9 is operated to enable the temperature control table 10 to reach the temperature T required by the generation of the hydrate1And keeping the temperature unchanged;
and 5: after the step 4 is finished, taking down the pressure-resistant injector 2 from the precise high-pressure injection pump 1 to suck enough 5 wt% of NaCl solution, opening the gas- liquid valves 3 and 15 after the NaCl solution is put back, operating the precise high-pressure injection pump 1 to enable the pressure-resistant injector 2 to simultaneously inject 5 wt% of NaCl solution to two ends of the pressure-resistant micro-fluidic glass chip 11 to increase pressure, observing the digital pressure gauge 8, and when the pressure reaches the pressure P required by hydrate generation2Then, the pressure-resistant injector 2 stops injecting by controlling the precise high-pressure injection pump 1, the gas- liquid valves 3, 7 and 15 are closed, timing is started, and the pressure gauge displays the pressure in the micropore of the pressure-resistant micro-fluidic glass chip 11;
step 6: after the step 5 is finished, closely paying attention to the numerical value of the digital pressure gauge 8, and when the pressure is from P2When the fast descending is started, the timing is stopped, at this time, CH4The induction time of the hydrate in 5 wt% NaCl solution is recorded as t1
And 7: after the step 6 is finished, opening the gas- liquid valves 3, 7 and 15 and the air release valve 14, injecting deionized water again through the pressure-resistant injector 2 to clean the pipeline and the pressure-resistant microfluidic glass chip 11, and properly collecting experimental waste gas and waste liquid;
and 8: after completion of step 7, the operations of steps 1 to 7 were repeated, but the solution initially charged in the pressure-resistant syringe 2 was changed to 10 wt% NaCl solution, and when the operation of step 2 was repeated, attention was paid to the suction of CH into the pressure-resistant syringe 24Is determined as V, and the outlet pressure of the gas cylinder is set as P1When the steps 4 and 5 are repeated, the readings of the temperature control table 10 and the digital pressure gauge 8 should be T1And P2And finally CH is obtained4The induction time of the hydrate in 5 wt% NaCl solution is recorded as t2The inhibitory effect of the two solutions can be compared by induction time.
Example 3:
the difference from example 1 is: the visual high-pressure microfluidic hydrate simulation experiment device is used for natural gas hydrate replacement exploitation experiments and uses CO2Replacement mining of CH4For example, with reference to fig. 1, the experimental procedure is as follows:
the pressure-resistant syringe 2 was initially filled with deionized water and the gas cylinder 5 with CH4The gas cylinder 6 is filled with CO2All valves are closed by default in the initial state;
step 1: opening gas- liquid valves 3 and 7 and an emptying valve 14, operating a precise high-pressure injection pump 1 to enable a pressure-resistant injector 2 to start injecting deionized water, and enabling micropores etched by a pressure-resistant micro-fluidic glass chip 11 to be completely filled with deionized water;
step 2: after the step 1 is finished, the precise high-pressure injection pump 1 is operated to stop the injection of the pressure-resistant injector 2, the gas-liquid valve 3 and the vent valve 14 are closed, the gas/liquid valve 4 and the gas bottle 5 are opened, and CH begins to be injected into the pressure-resistant micro-fluidic glass chip 114Gas, small amount of CH injected4After gas (hydrate can be completely generated), closing the gas-liquid valve 4 and the gas bottle 5;
and step 3: after the step 2 is finished, the micro cooling pump 9 is operated to enable the temperature control table 10 to reach the temperature T required by the generation of the hydrate1And keeping the temperature unchanged;
and 4, step 4: after the step 3 is finished, opening the gas- liquid valves 3 and 15, operating the precise high-pressure injection pump 1 to enable the pressure-resistant injector 2 to simultaneously inject deionized water to two ends of the pressure-resistant micro-fluidic glass chip 11 to increase the pressure, observing the digital pressure gauge 8, and when the pressure reaches the pressure P required by hydrate generation1Then, the pressure-resistant injector 2 stops injecting by controlling the precise high-pressure injection pump 1, and the gas- liquid valves 3, 7 and 15 are closed;
and 5: after step 4 is completed, measuring CH in the microporosity in real time by using image processing software carried by an optical phase contrast microscope 12 and a computer 134Volume V of micro-pores occupied by gas1And observe CH4The process of hydrate gradual formation until the hydrate form is not changed;
step 6: after the step 5 is finished, opening the gas- liquid valves 4, 7 and 16 and the gas cylinder 6, and starting to move to the pressure-resistant micro-fluidic glassContinuous CO injection into the chip 112Gas and adjusting corresponding valve to stabilize the reading of the digital pressure gauge at P2And starting to record the experimental time t;
and 7: after step 6 is completed, real-time observation and recording of CO are carried out by image processing software carried by the optical phase contrast microscope 12 and the computer 132Substitution of CH4In the process of hydrate, after a gas-liquid mixture generated by the simultaneous reaction is dried by a drying device 17, the flow rate Q and the volume V of the drying gas are measured by a gas micro-flow meter 18 at room temperature T0Standard atmospheric pressure P0Measured under the conditions, collected in a gas collecting device 19, and the gas components generated by the reaction can be detected by a gas chromatograph to obtain CH4Volume fraction of gas occupied
Figure BDA0002375089530000071
At the experimental time t, with the pressure P2Continuous CO injection2Gas replacement of CH4Production efficiency K (CH produced) obtained for hydrate4In an amount corresponding to CH forming hydrate4Ratio of amounts) is:
Figure BDA0002375089530000081
and 8: and (7) after the step (7) is finished, opening the gas/liquid valves (3, 7 and 15) and the emptying valve (14), closing the gas/liquid valve (16), injecting deionized water again through the pressure-resistant injector (2) to clean the pipeline and the pressure-resistant microfluidic glass chip (11), and properly collecting experimental waste gas and waste liquid.
The above description is only an example of the present invention, and is not intended to limit the present invention in any way, and those skilled in the art can make many variations and modifications of the present invention without departing from the scope of the present invention by using the method disclosed above, and the present invention is covered by the claims.

Claims (8)

1. The utility model provides a visual high pressure micro-fluidic hydrate simulation experiment device which characterized in that: the device comprises a micro-fluid injection and pressure control unit, a pressure-resistant micro-fluidic hydrate reaction unit, a temperature control unit, a generated gas processing unit and a real-time display unit, wherein the micro-fluid injection and pressure control unit quantitatively injects gas or solution to a pressure-resistant micro-fluidic chip where a hydrate is located and adjusts the pressure in the chip where the hydrate reacts; the pressure-resistant microfluidic hydrate reaction unit mainly comprises a plurality of pressure-resistant microfluidic glass chips; the temperature control unit controls the temperature of the chip where the hydrate reaction is located; the generated gas processing unit dries a product in the hydrate reaction process, measures the flow of a gas product, and collects reaction gas; the real-time display unit observes the reaction process of the hydrate in the micropores of the pressure-resistant glass chip in real time, and all units are connected through pipelines or data lines and controlled through corresponding valves or switches.
2. The visual high-pressure microfluidic hydrate simulation experiment device according to claim 1, wherein: the micro-fluid injection and pressure control unit comprises a precise high-pressure injection pump, a pressure-resistant injector and a digital pressure gauge, wherein the precise high-pressure injection pump controls the pressure-resistant injector to inject gas or solution into the pressure-resistant micro-fluidic hydrate reaction unit, and the digital pressure gauge displays the pressure of a corresponding pipeline in real time.
3. The visual high-pressure microfluidic hydrate simulation experiment device according to claim 1 or 2, wherein: the micro-fluid injection and pressure control unit also comprises a plurality of gas cylinders with regulating valves and a plurality of regulating valves, wherein the gas cylinders supply gas to the pressure-resistant injector, and the regulating valves regulate the liquid injection speed to control the pressure of the hydrate reaction.
4. The visual high-pressure microfluidic hydrate simulation experiment device according to claim 1, wherein: the pressure-resistant microfluidic glass chip of the pressure-resistant microfluidic hydrate reaction unit is connected with the temperature control unit through a clamp and is connected with the micro-fluid injection and pressure control unit through a stainless steel pipeline and a joint.
5. The visual high-pressure microfluidic hydrate simulation experiment device according to claim 1, wherein: the temperature control unit comprises a temperature control table and a micro cooling pump connected with the temperature control table through a heat insulation pipeline, wherein the micro cooling pump cools the temperature control table through setting the temperature of circulating cooling liquid, and the temperature control table is heated through an internal semiconductor.
6. The microfluidic experimental device for visualizing high-pressure hydrate reaction according to claim 1, wherein: the generated gas processing unit comprises a drying device, a gas micro-flow meter and a gas collecting device, wherein the drying device is used for drying a gas-liquid mixture generated in the hydrate reaction process, the gas flow meter is used for measuring the real-time flow and the accumulated flow in the hydrate reaction process, and the gas collecting device is used for collecting gas generated in the hydrate reaction process.
7. The visual high-pressure microfluidic hydrate simulation experiment device according to claim 1, wherein: the real-time display unit comprises an optical phase difference microscope, a computer and corresponding image processing software, the optical phase difference microscope is used for observing the reaction behavior of the hydrate in the micropore and displaying the phase interface of the hydrate-gas-liquid three phase, the optical phase difference microscope is connected with the computer through a data line, and the corresponding image processing software in the computer can obtain the microscopic form of the hydrate in the pressure-resistant micro-fluidic glass chip in real time.
8. The application of a visual high-pressure microfluidic hydrate simulation experiment device in simulation of hydrate generation and decomposition experiments in formation micropores, evaluation of effect of hydrate inhibitor solution and replacement and exploitation of natural gas hydrates is provided.
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CN115078356A (en) * 2022-05-20 2022-09-20 西南石油大学 High-temperature high-pressure condensate gas phase state micro-fluidic experimental method in porous medium
CN116046778A (en) * 2023-03-06 2023-05-02 西南石油大学 On-line visual test equipment and method for hydrate generation and inhibition effect
CN117723116A (en) * 2023-12-15 2024-03-19 东北石油大学三亚海洋油气研究院 Device and method for researching microcosmic residual oil in nanoscale pore canal

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103233704A (en) * 2013-05-01 2013-08-07 吉林大学 Method and device for simulating experiment of permafrost region natural gas hydrate mining through replacement of CO2/N2
CN103792170A (en) * 2012-11-01 2014-05-14 中国石油化工股份有限公司 Simulation experiment device system for porous medium microscopic seepage
US20160299047A1 (en) * 2013-11-21 2016-10-13 Schlumberger Technology Corporation Method and apparatus for characterizing clathrate hydrate formation conditions employing microfluidic device
CN206248502U (en) * 2016-12-03 2017-06-13 中国计量大学 A kind of photomicrography experimental provision on soft particle rheological behavior
CN106969957A (en) * 2017-04-20 2017-07-21 天津大学 A kind of Multifunctional, air gas hydrate experimental system
CN107632134A (en) * 2017-10-23 2018-01-26 大庆东油睿佳石油科技有限公司 A kind of gas hydrates seawater drives photoetching glass model microcosmos experiment device
CN108195647A (en) * 2017-12-30 2018-06-22 北京化工大学 It is a kind of simulate oil reservoir miniature model and carry out the method for petroleum driving experiment with it
CN109209359A (en) * 2018-08-01 2019-01-15 中国石油大学(华东) Gas hydrates drilling microcosmic Simulation device

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103792170A (en) * 2012-11-01 2014-05-14 中国石油化工股份有限公司 Simulation experiment device system for porous medium microscopic seepage
CN103233704A (en) * 2013-05-01 2013-08-07 吉林大学 Method and device for simulating experiment of permafrost region natural gas hydrate mining through replacement of CO2/N2
US20160299047A1 (en) * 2013-11-21 2016-10-13 Schlumberger Technology Corporation Method and apparatus for characterizing clathrate hydrate formation conditions employing microfluidic device
CN206248502U (en) * 2016-12-03 2017-06-13 中国计量大学 A kind of photomicrography experimental provision on soft particle rheological behavior
CN106969957A (en) * 2017-04-20 2017-07-21 天津大学 A kind of Multifunctional, air gas hydrate experimental system
CN107632134A (en) * 2017-10-23 2018-01-26 大庆东油睿佳石油科技有限公司 A kind of gas hydrates seawater drives photoetching glass model microcosmos experiment device
CN108195647A (en) * 2017-12-30 2018-06-22 北京化工大学 It is a kind of simulate oil reservoir miniature model and carry out the method for petroleum driving experiment with it
CN109209359A (en) * 2018-08-01 2019-01-15 中国石油大学(华东) Gas hydrates drilling microcosmic Simulation device

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
关进安等: "一套模拟渗漏型天然气水合物形成与分解的实验***", 《天然气工业》 *

Cited By (15)

* Cited by examiner, † Cited by third party
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CN111735813A (en) * 2020-07-20 2020-10-02 大连理工大学 Experimental device for generating micro-bubbles and promoting generation of hydrate by applying micro-fluidic chip
CN112461837A (en) * 2020-11-05 2021-03-09 东北石油大学 Hydrate synthesis and decomposition visual experimental device
CN112858113A (en) * 2021-01-08 2021-05-28 中国石油大学(华东) Microscopic visual experimental method for high-temperature high-pressure gas flooding of deep reservoir
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WO2022156052A1 (en) * 2021-01-22 2022-07-28 中国石油大学(华东) Microfluidic chip experimental platform having visualization and infrared thermal imaging functions
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CN113358703A (en) * 2021-06-16 2021-09-07 中国石油大学(华东) Micro-scale experimental device and method for simulating hydrate phase change under electric field condition
CN115032122A (en) * 2022-03-29 2022-09-09 哈尔滨工程大学 Device and method for measuring evolution characteristic of hydrate permeability based on microfluidic model
CN115078356A (en) * 2022-05-20 2022-09-20 西南石油大学 High-temperature high-pressure condensate gas phase state micro-fluidic experimental method in porous medium
CN116046778A (en) * 2023-03-06 2023-05-02 西南石油大学 On-line visual test equipment and method for hydrate generation and inhibition effect
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