CN102243183A - Experimental device for in-situ monitoring of hydrate phase equilibrium - Google Patents
Experimental device for in-situ monitoring of hydrate phase equilibrium Download PDFInfo
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- CN102243183A CN102243183A CN2011100864683A CN201110086468A CN102243183A CN 102243183 A CN102243183 A CN 102243183A CN 2011100864683 A CN2011100864683 A CN 2011100864683A CN 201110086468 A CN201110086468 A CN 201110086468A CN 102243183 A CN102243183 A CN 102243183A
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Abstract
The invention relates to a test device, and especially relates to an experimental device for in-situ monitoring of hydrate phase equilibrium. The experimental device is characterized in that the device comprises a housing body; a reaction vessel and a gas storage container are arranged in the housing body and are communicated with each other by a gas feed pipe; the gas storage container is communicated with a gas bomb by a gas feed pipe and a pressure device; the reaction vessel is connected with a computer microprocessor through an optical imaging system, a metering control system and a chromatographic analysis system; and the reaction vessel is arranged in a water-bath jacket. Based on the experimental device, during the whole experiment process, the in-situ real-time recording of temperature data, pressure data, image data and chromatographic analysis data is carried out in one device by a computer system.
Description
Technical field
The present invention relates to a kind of proving installation, relate in particular to a kind of hydrate phase balance in-situ monitoring experimental provision.
Background technology
The generation of gas hydrate and decomposable process are actually the process that " hydrate-water-rock gas " three-phase equilibrium changes, and the factor that any influence balances each other can both influence the generation and the decomposable process of gas hydrate.Therefore, study " hydrate-water-rock gas " condition of three-phase balance and influence factor thereof under the various conditions, can obtain the generation and the decomposed information of gas hydrate.
The monitoring function of the hydrate phase balance emulation experiment device of having reported at present both at home and abroad is uneven, attend to one thing and lose sight of another, not to be difficult to the Direct observation experimental phenomena, be exactly less and the online on-line working of modern precision monitoring instrument, and multi-functional while in-situ monitoring technology is deficient especially.Therefore,, be difficult to while research experiment influence factor on the multiparameter level, be difficult to original position and obtain high-precision gas composition differentiation data and high-resolution growth, extinction behavior image in real time at the research that balances each other of multicomponent gas hydrate.
Summary of the invention
Technique effect of the present invention can overcome above-mentioned defective, and a kind of hydrate phase balance in-situ monitoring experimental provision is provided, and it is simple in structure, good test effect.
For achieving the above object, the present invention adopts following technical scheme: it comprises housing, is provided with the reactor and the air container that are interconnected by steam line in the housing, and air container is communicated with gas bomb by steam line, pressue device; Reactor is connected with computer microprocessor by imaging fiber system, metering control system, chromatographic analysis system respectively; Reactor is arranged in the water-bath chuck.
But its core application technology of the experimental provision of this invention is the gas composition situation in the simulating nature geologic condition, and the phase balance condition of research multicomponent gas hydrate can carry out original position to experiment parameter simultaneously multi-functionally and monitor in real time.Imaging fiber system: generation and the decomposition behavior that can observe and write down hydrate in real time, intuitively and accurately; Chromatographic analysis system: when research multicomponent gas hydrate phase balance condition, but each gas composition of in-situ monitoring and water reaction form the ability of hydrate, and the relative content of each gas composition changes in the hydrate formation/decomposable process; Control system: controller adopts PID voltage stabilizing Control Component and pneumatic valve Control Component, is controlled in real time by computing machine, and the gaseous tension of air container supply response still is controlled, and can accurately control the air inflow of reactor.This invention is used for the multiparameter while in-situ monitoring of multicomponent gas hydrate phase balance research in the laboratory.The main core technology of device has been to design the autoclave of band transparent window, has introduced accurate optical fiber imaging system, has realized the online online detection technique of chromatogram, and monitoring means is more abundant simultaneously, and pressurize is quick and convenient automatically, and visual degree is higher.This device is the generation and the decomposition behavior of Real Time Observation, record multicomponent gas hydrate intuitively and accurately, but the differentiation trend of each gas composition in the in-situ monitoring hydrate formation/decomposable process helps carrying out from the multiparameter level research that balances each other of multicomponent gas hydrate.
The bottom of reactor is provided with magnetic stirring apparatus.Mode by magnetic agitation drives rotor, thereby stirs liquid in the still, can stir under the situation of not disturbance liquid-gas interface, can effectively avoid the requirement of mechanical type stirring to high pressure sealing.
Steam line between reactor and the air container is provided with the PID controller.Reactor inside is provided with two temperature sensors, and one of them is positioned at the upside of reactor inside, and another is positioned at the downside of reactor inside.The reactor top is provided with vacuum lead, and vacuum lead is communicated with steam line, and vacuum lead is provided with pressure transducer, safety valve, and vacuum lead is communicated with metering control system.
The side of reactor is provided with transparent visual window.Autoclave band transparent window, integral body is quick-opening structure, the kettle outside is furnished with the water-bath chuck, can accurately control experimental temperature in the still;
The reactor top is provided with sampling conduit, and sampling conduit is communicated with chromatographic analysis system by valve.Air container is provided with vacuum lead, and vacuum lead is communicated with steam line, and vacuum lead is provided with safety valve.Air container is provided with pressure transducer.
Adopt the hydrate phase balance in-situ monitoring experimental provision of this structure, can be in same device, in whole experiment, data such as temperature, pressure, image, stratographic analysis are by computer system original position real time record.Can intuitively observe the generation/decomposition behavior of hydrate according to image data, can accurately monitor the response situation of each gas composition, can draw the phase balance condition of multicomponent gas hydrate in conjunction with temperature, pressure monitoring value according to chromatogram analysis data.
Description of drawings
Below in conjunction with the drawings and specific embodiments the present invention is done detailed description:
Fig. 1 is an one-piece construction synoptic diagram of the present invention.
Among the figure: 1. housing; 2. reactor; 3. air container; 4. gas bomb; 5. chromatographic analysis system; 6. metering control system; 7. imaging fiber system; 8. computer microprocessor; 9. magnetic stirring apparatus; 10.PID controller; 11. valve; 12. temperature sensor; 13. vacuum lead; 14. steam line; 15. pressure transducer; 16. safety valve; 17. visual window; 18. water-bath chuck; 19. pressue device; 20. sampling conduit.
Embodiment
Experimental provision of the present invention comprises housing 1, is provided with the reactor 2 and the air container 3 that are interconnected by steam line 14 in the housing 1, and air container 3 is communicated with gas bomb 4 by steam line 14, pressue device 19; Reactor 2 is connected with computer microprocessor 8 by imaging fiber system 7, metering control system 6, chromatographic analysis system 5 respectively; Reactor 2 is arranged in the water-bath chuck 18.
The bottom of reactor 2 is provided with magnetic stirring apparatus 9.Steam line 14 between reactor 2 and the air container 3 is provided with PID controller 10.Reactor inside is provided with two temperature sensors 12, and one of them is positioned at the upside of reactor inside, and another is positioned at the downside of reactor inside.The reactor top is provided with vacuum lead 13, and vacuum lead 13 is communicated with steam line 14, and vacuum lead 13 is provided with pressure transducer 15, safety valve 16, and vacuum lead 13 is communicated with metering control system 6.The side of reactor is provided with transparent visual window 17.The reactor top is provided with sampling conduit 20, and sampling conduit 20 is communicated with chromatographic analysis system 5 by valve 11.Air container 3 is provided with vacuum lead 13, and vacuum lead 13 is communicated with steam line 14, and vacuum lead 13 is provided with safety valve 16.Air container 3 is provided with pressure transducer 15.
In the experimental provision of this invention, the top pressure of reactor 2 is 20MPa, and the top pressure of air container 3 is 30MPa, is respectively applied for the synthetic and work such as decomposition, supercharging and decompression of hydrate.Two temperature sensors 12 are arranged in reactor 2, measure the temperature of still internal upper part gas and the temperature of lower liquid respectively, measuring accuracy is ± 0.1 ℃.The pressure of reactor 2 is by 10 controls of PID controller, and by a pressure transducer 15 measurement reactors 2 internal pressures that are connected on the reactor, pressure measurement accuracy is ± 0.1Mpa.Temperature control system is formed (temperature range-20-50 ℃) by constant temperature oven and built-in cryogenic thermostat water-bath equipment, mainly cooperate constant temperature ovens to come temperature in the conditioned reaction still in the experiment by reactor water-bath chuck 18, by reducing temperature hydrate is generated, the temperature that raises subsequently makes decomposition of hydrate.Data (comprising temperature, pressure, image, stratographic analysis etc.) all in the experimentation are gathered and record in real time by computer system.
Multicomponent gas hydrate phase balance research in-situ monitoring experimental procedure is as follows:
1, checks at first whether device lines such as all pipelines, circuit are normal, open the power supply of central microprocessor, chromatographic analysis system, imaging fiber system, metering control system again, and start experiment software, chromatographic work station, imaging video software;
2, enter experiment software and begin image data, whether the experimental data of observing each passage is normal, and by relevant control knob, whether check PID variable valve and operated pneumatic valve be working properly;
3, open the fujinon electronic video endoscope of imaging system, each circuit is connected normally, see normally images acquired or video;
4, check chromatographic analysis system, guarantee that each position is working properly, the stratographic analysis parameter is set, treat stand-by operation after the baseline stability;
5, begin experiment before, earlier reactor is cleaned up, the high purity water that reinjects is built reactor to having an X-rayed the window medium position, checks and guarantees that each connecting portion is all fastening firm;
6, utilize pumped vacuum systems, whole experiment container and pipeline are vacuumized, the air that retains with emptying internal system (comprising water);
7, open the pressurization gas distributing system, in reactor, feed experimental gas by air container, make reacting kettle inner pressure reach the pressure of experimental design, each connecting portion is carried out airtight test, balance and stability a period of time, can or regulate rotating speed according to experiment needs determine switch magnetic stirring apparatus;
8, the temperature that reduces constant temperature oven and water-bath to the experimental design temperature to generate gas hydrate, treat that hydrate generates and balance stops temperature control after a period of time, bath temperature is risen, hydrate can decompose;
9, in hydrate generation/decomposable process, can carry out the real-time video shooting to overall process by imaging device, but, but change by the relative content of still internal reaction gas of arbitrary moment of gas chromatography on-line analysis or each component of decomposition of hydrate gas by pressure, temperature sensor The real time measure still internal pressure, gas and fluid temperature;
10, during stratographic analysis, need still internal upper part gas is imported in the pipeline between valve, this moment still internal pressure about 0.03-0.06Mpa that descends, this pressure drop does not influence the interior reflex action of still in experimental pressure allows fluctuation range.The test gas that pipeline is suppressed between valve will import chromatograph analysis automatically by the gas chromatographic valve sampling device, can supply 6 usefulness of parallel analysis, satisfy the requirement of chromatogram replicate determination fully;
11, in the whole experiment, data such as temperature, pressure, image, stratographic analysis are by computer system original position real time record.Can intuitively observe the generation/decomposition behavior of hydrate according to image data, can accurately monitor the response situation of each gas composition, can draw the phase balance condition of multicomponent gas hydrate in conjunction with temperature, pressure monitoring value according to chromatogram analysis data.
Claims (9)
1. hydrate phase balance in-situ monitoring experimental provision, it is characterized in that, comprise housing (1), be provided with the reactor (2) and the air container (3) that are interconnected by steam line (14) in the housing (1), air container (3) is communicated with gas bomb (4) by steam line (14), pressue device (19); Reactor (2) is connected with computer microprocessor (8) by imaging fiber system (7), metering control system (6), chromatographic analysis system (5) respectively; Reactor (2) is arranged in the water-bath chuck (18).
2. hydrate phase balance in-situ monitoring experimental provision according to claim 1 is characterized in that the bottom of reactor (2) is provided with magnetic stirring apparatus (9).
3. hydrate phase balance in-situ monitoring experimental provision according to claim 2 is characterized in that, the steam line (14) between reactor (2) and the air container (3) is provided with PID controller (10).
4. hydrate phase balance in-situ monitoring experimental provision according to claim 2 is characterized in that reactor inside is provided with two temperature sensors (12), and one of them is positioned at the upside of reactor inside, and another is positioned at the downside of reactor inside.
5. hydrate phase balance in-situ monitoring experimental provision according to claim 4, it is characterized in that, the reactor top is provided with vacuum lead (13), vacuum lead (13) is communicated with steam line (14), vacuum lead (13) is provided with pressure transducer (15), safety valve (16), and vacuum lead (13) is communicated with metering control system (6).
6. hydrate phase balance in-situ monitoring experimental provision according to claim 4 is characterized in that the side of reactor is provided with transparent visual window (17).
7. hydrate phase balance in-situ monitoring experimental provision according to claim 2 is characterized in that the reactor top is provided with sampling conduit (20), and sampling conduit (20) is communicated with chromatographic analysis system (5) by valve (11).
8. hydrate phase balance in-situ monitoring experimental provision according to claim 2, it is characterized in that, air container (3) is provided with vacuum lead (13), and vacuum lead (13) is communicated with steam line (14), and vacuum lead (13) is provided with safety valve (16).
9. hydrate phase balance in-situ monitoring experimental provision according to claim 8 is characterized in that air container (3) is provided with pressure transducer (15).
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103196861A (en) * | 2013-03-29 | 2013-07-10 | 西安交通大学 | Flowing high temperature and high pressure phase equilibrium measuring device and application method thereof |
| CN103257203A (en) * | 2012-02-16 | 2013-08-21 | 中国科学院物理研究所 | High-pressure integrated experiment apparatus for novel energy hydrate |
| CN103308518A (en) * | 2013-05-22 | 2013-09-18 | 中国航天科技集团公司第六研究院第十一研究所 | Heavy-piston quick pressure testing system and method for realizing supercritical state by utilizing same |
| CN104227011A (en) * | 2014-08-29 | 2014-12-24 | 南京邮电大学 | Device for preparing nano-metallic material in macroscopic amount and preparation method for nano-metallic material |
| CN108983846A (en) * | 2018-06-21 | 2018-12-11 | 南方电网科学研究院有限责任公司 | A kind of investigating method of medium parameter |
| CN109507063A (en) * | 2018-10-30 | 2019-03-22 | 黑龙江科技大学 | Multicomponent Gas Hydrate variable volume phase balance determining device |
| CN109540763A (en) * | 2018-12-10 | 2019-03-29 | 青岛海洋地质研究所 | The sample preparation and transfer device and method of hydrate CT and SEM joint test |
| CN110554038A (en) * | 2019-07-17 | 2019-12-10 | 华南理工大学 | device and method capable of realizing synchronous mesoscopic observation of formation and decomposition of gas hydrate |
| CN111889052A (en) * | 2020-07-20 | 2020-11-06 | 常州大学 | Hydrate decomposition experimental device capable of automatically adding liquid |
| CN112619558A (en) * | 2020-12-10 | 2021-04-09 | 中国海洋石油集团有限公司 | Device and method for observing in-situ growth form of hydrate crystal at multiple viewing angles |
| CN114288969A (en) * | 2021-12-28 | 2022-04-08 | 江苏华安科研仪器有限公司 | Rodless large visual phase equilibrium hydrate reactor |
| WO2023279859A1 (en) * | 2021-07-09 | 2023-01-12 | 齐鲁工业大学 | Device for monitoring gas hydrate generation and decomposition process at molecular level in-situ by using online infrared spectrometer, and use method of same |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103257203A (en) * | 2012-02-16 | 2013-08-21 | 中国科学院物理研究所 | High-pressure integrated experiment apparatus for novel energy hydrate |
| CN103196861A (en) * | 2013-03-29 | 2013-07-10 | 西安交通大学 | Flowing high temperature and high pressure phase equilibrium measuring device and application method thereof |
| CN103196861B (en) * | 2013-03-29 | 2014-12-10 | 西安交通大学 | Flowing high temperature and high pressure phase equilibrium measuring device and application method thereof |
| CN103308518A (en) * | 2013-05-22 | 2013-09-18 | 中国航天科技集团公司第六研究院第十一研究所 | Heavy-piston quick pressure testing system and method for realizing supercritical state by utilizing same |
| CN104227011A (en) * | 2014-08-29 | 2014-12-24 | 南京邮电大学 | Device for preparing nano-metallic material in macroscopic amount and preparation method for nano-metallic material |
| CN108983846A (en) * | 2018-06-21 | 2018-12-11 | 南方电网科学研究院有限责任公司 | A kind of investigating method of medium parameter |
| CN109507063A (en) * | 2018-10-30 | 2019-03-22 | 黑龙江科技大学 | Multicomponent Gas Hydrate variable volume phase balance determining device |
| CN109540763A (en) * | 2018-12-10 | 2019-03-29 | 青岛海洋地质研究所 | The sample preparation and transfer device and method of hydrate CT and SEM joint test |
| CN109540763B (en) * | 2018-12-10 | 2019-08-06 | 青岛海洋地质研究所 | The sample preparation and transfer device and method of hydrate CT and SEM joint test |
| CN110554038A (en) * | 2019-07-17 | 2019-12-10 | 华南理工大学 | device and method capable of realizing synchronous mesoscopic observation of formation and decomposition of gas hydrate |
| CN110554038B (en) * | 2019-07-17 | 2022-02-25 | 华南理工大学 | Device and method capable of realizing synchronous mesoscopic observation of formation and decomposition of gas hydrate |
| CN111889052A (en) * | 2020-07-20 | 2020-11-06 | 常州大学 | Hydrate decomposition experimental device capable of automatically adding liquid |
| CN112619558A (en) * | 2020-12-10 | 2021-04-09 | 中国海洋石油集团有限公司 | Device and method for observing in-situ growth form of hydrate crystal at multiple viewing angles |
| WO2023279859A1 (en) * | 2021-07-09 | 2023-01-12 | 齐鲁工业大学 | Device for monitoring gas hydrate generation and decomposition process at molecular level in-situ by using online infrared spectrometer, and use method of same |
| CN114288969A (en) * | 2021-12-28 | 2022-04-08 | 江苏华安科研仪器有限公司 | Rodless large visual phase equilibrium hydrate reactor |
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Application publication date: 20111116 |