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CN112452277A - Hydrate formation experimental apparatus under influence of memory effect - Google Patents

Hydrate formation experimental apparatus under influence of memory effect Download PDF

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Publication number
CN112452277A
CN112452277A CN202011276393.0A CN202011276393A CN112452277A CN 112452277 A CN112452277 A CN 112452277A CN 202011276393 A CN202011276393 A CN 202011276393A CN 112452277 A CN112452277 A CN 112452277A
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ball valve
memory effect
influence
temperature
hydrate
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敬加强
杨航
罗佳琪
程原招
张兴堂
王海燕
石运亮
付斌
郭雨莹
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Southwest Petroleum University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00

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Abstract

本发明公开一种记忆效应影响下水合物生成实验装置,该装置通过提前制备具有一次水合物生成历史水相的方法,将具有一次和二次水合物生成历史的记忆效应影响下的水合物生成实验的实验次数从n+n+n次减少为1+n+n次。本发明提供的记忆效应影响下水合物生成实验装置和方法,可减少实验次数和实验时间,提高实验效率。

Figure 202011276393

The invention discloses an experimental device for hydrate generation under the influence of memory effect. The device uses a method for preparing a water phase with a history of primary hydrate generation in advance, and the device generates hydrate under the influence of memory effect with primary and secondary hydrate generation history. The number of experiments was reduced from n+n+n to 1+n+n. The experimental device and method for hydrate generation under the influence of memory effect provided by the invention can reduce the number of experiments and the experiment time and improve the experiment efficiency.

Figure 202011276393

Description

Hydrate formation experimental apparatus under influence of memory effect
Technical Field
The invention relates to a gas hydrate generation simulation experiment device, in particular to an experiment device and method for predicting hydrate generation time under the influence of memory effect.
Background
The gas hydrate needs to be prepared for nucleation before visible crystallization occurs, and the change of the system characteristics cannot be observed by naked eyes in the preparation process, which is called induction phenomenon, and the preparation time is called induction time. The hydrate is regenerated in the water phase with the history of hydrate generation, the induction period of hydrate generation is obviously shortened, the phenomenon is the memory effect of hydrate generation, and the induction period of the hydrate with the history of secondary generation is shorter than that of the hydrate with the history of primary generation. At present, the experimental measurement related to the memory effect generally adopts a method that a hydrate generation experiment is firstly carried out, then the temperature is increased to decompose the hydrate, and then a second hydrate generation experiment is carried out under the condition of keeping the same working condition as the previous experiment. Therefore, if only the influence of the memory effect on the generation of the hydrate needs to be analyzed, a set of data is measured, two experiments need to be carried out, and particularly for the experiment of generating the hydrate of the oil-containing system, because the mixing of an oil-gas-water three-phase experiment medium is involved, the memory effect of the hydrate generation can be analyzed in the second experiment after the first experiment of generating the hydrate is carried out, so the experiment amount is large, the time for generating the hydrate in the water phase without the history of generating the hydrate is long, namely the experiment time of the first experiment of generating the hydrate accounts for a large proportion in the whole experiment. From this, need design hydrate formation experimental apparatus under the memory effect influence in order to reduce the experiment number of times, reduce the experimental time, promote experimental efficiency.
Disclosure of Invention
Aiming at the technical problems, the invention provides a hydrate generation experimental device and method under the influence of memory effect so as to reduce the experimental times and improve the experimental efficiency.
The technical scheme adopted by the invention is as follows:
an experimental device for generating hydrates under the influence of a memory effect comprises a high-pressure reaction kettle (1), a gas supply system (2), a liquid supply system (3), a water storage device (4), an oil storage device (5), a gas storage device (6), a three-phase separator (7), a centrifugal pump (8), a first ball valve (9), a second ball valve (10), a third ball valve (11), a fourth ball valve (12), a fifth ball valve (13), a sixth ball valve (14), a first temperature transmitter (15), a second temperature transmitter (16), a pressure transmitter (17), a temperature control system (18), a magnetic stirrer (19), a flowmeter (20), a vacuum pump (21), a safety valve (22), a temperature and pressure acquisition system (23), a computer (24), a seventh ball valve (25), an eighth ball valve (26) and a ninth ball valve (27).
The gas supply system (2) and the liquid supply system (3) respectively inject experimental gas and liquid into the high-pressure reaction kettle (1), and the temperature control system (18) is used for controlling the temperature of experimental media in the high-pressure reaction kettle (1).
Wherein the high-pressure reaction kettle (1) is provided with a visual window.
Wherein, the safety valve (22) is connected with the high-pressure reaction kettle (1) and is used for controlling the pressure in the high-pressure reaction kettle (1) and ensuring the safe operation of the experiment. The experimental device for generating the hydrate under the influence of the memory effect has the advantages that the experimental device for generating the hydrate under the influence of the memory effect can prepare water with reaction history required by the memory effect experiment and store the water in the liquid storage device (4), then the water in the liquid storage device (4) is pumped to the liquid supply system (3), through the means, the experimental process is improved into the method that the water phase with the history of generating the hydrate is prepared firstly, then the induction time under the influence of the memory effect of generating the hydrate can be measured by controlling variables to carry out the experiment, and if the experimental device is used for carrying out the experiment that the wax-containing oil gas system influences the generation of the hydrate under the influence of the memory effect with the history of generating the primary hydrate and the memory effect of generating the secondary hydrate, 15(5+5+5) groups of experiments can be reduced into 11(1+5+5) groups.
Drawings
FIG. 1 is a schematic structural diagram of an experimental apparatus for generating hydrates under the influence of memory effect.
In the figure, 1-a high-pressure reaction kettle, 2-a gas supply system, 3-a liquid supply system, 4-a water storage device, 5-an oil storage device, 6-a gas storage device, 7-a three-phase separator, 8-a centrifugal pump, 9-a first ball valve, 10-a second ball valve, 11-a third ball valve, 12-a fourth ball valve, 13-a fifth ball valve, 14-a sixth ball valve, 15-a first temperature transmitter, 16-a second temperature transmitter, 17-a pressure transmitter, 18-a temperature control system, 19-a magnetic stirrer, 20-a flow meter, 21-a vacuum pump, 22-a safety valve, 23-a temperature and pressure acquisition system, 24-a computer, 25-a seventh ball valve, 26-an eighth ball valve and 27-a ninth ball valve.
Detailed Description
Fig. 1 is a schematic structural diagram of a hydrate formation experimental apparatus under the influence of a memory effect, taking an example of an experiment of influence of different wax contents on hydrate formation under the influence of a memory effect with a history of primary and secondary hydrate formation of a wax-containing oil gas system, the working process of the experiment is as follows:
1. preparation of aqueous phase with history of primary hydrate formation: the temperature control system (18) is set to the temperature required for the experiment before the experiment begins. And opening the fifth ball valve (13), opening the vacuum pump (21), and closing the vacuum pump (21) and the fifth ball valve (13) when the pressure in the high-pressure reaction kettle (1) reaches-0.08 MPa. And opening the second ball valve (10), injecting deionized water into the high-pressure reaction kettle (1) through the liquid supply system (3), and closing the second ball valve (10) after injection is completed. After the temperature of deionized water in the high-pressure reaction kettle (1) reaches the experiment temperature, a first ball valve (9) is opened, the methane gas required by the experiment is injected into the high-pressure reaction kettle (1) through a gas supply system (2), and when the pressure in the high-pressure reaction kettle (1) reaches the experiment pressure, the first ball valve (9) is closed, and a magnetic stirrer (19) is opened. And observing sudden temperature rise or sudden pressure drop of the system, observing that a large amount of hydrate is generated through a visual window of the high-pressure reaction kettle (1), regarding the moment as the end moment of the hydrate induction period, and closing the magnetic stirrer (19). And setting a temperature control system (18) to control the temperature to 60 ℃, standing to observe that the hydrate is completely decomposed, starting a sixth ball valve (14), putting gas and liquid in the high-pressure reaction kettle (1) into a three-phase separator (7) for gas-water separation, starting a third ball valve (11) and a seventh ball valve (25), recovering methane into a gas storage device (6), and recovering water into a water storage device (4). And (3) cleaning the high-pressure reaction kettle (1), and finishing the preparation of the experimental water.
2. Experiment of influence of different wax contents on hydrate formation under the influence of memory effect with history of primary and secondary hydrate formation: the temperature control system (18) is set to the temperature required for the experiment before the experiment begins. And opening the fifth ball valve (13), opening the vacuum pump (21), and closing the vacuum pump (21) and the fifth ball valve (13) when the pressure in the high-pressure reaction kettle (1) reaches-0.08 MPa. Open centrifugal pump (8) after eighth ball valve (26), open ninth ball valve (27) after slightly suppressing the pressure and pour into liquid supply system (3) with water storage device (4) partial water according to the demand into, and pour into liquid supply system (3) with the white oil that wax content is 3%, open second ball valve (10), pour into experimental liquid into high-pressure reaction cauldron (1) through liquid supply system (3), close second ball valve (10) after the completion of the injection, after the experiment liquid temperature reaches experimental temperature in high-pressure reaction cauldron (1), open first ball valve (9), through gas supply system (2) with the required methane gas injection high-pressure reaction cauldron (1) of experiment, when high-pressure reaction cauldron (1) internal pressure reached experimental pressure, close first ball valve (9), open magnetic stirrers (19). The temperature and pressure acquisition system (23) acquires the temperature and pressure in the high-pressure reaction kettle (1) in real time and stores the temperature and pressure in the computer (24), the temperature sudden rise or the pressure sudden fall of the system is observed, the generation of a large amount of hydrates can be observed through a visual window of the high-pressure reaction kettle (1), the moment is regarded as the end moment of the hydrate induction period, and the magnetic stirrer (19) is closed. And setting a temperature control system (18) to control the temperature to 60 ℃, standing to observe that the hydrate is completely decomposed, setting the temperature control system (18) to be the temperature required by the experiment, and starting a magnetic stirrer (19) after the experiment temperature is reached. And observing sudden temperature rise or sudden pressure drop of the system, observing that a large amount of hydrate is generated through a visual window of the high-pressure reaction kettle (1), regarding the moment as the end moment of the hydrate induction period, and closing the magnetic stirrer (19). And setting a temperature control system (18) to control the temperature to 60 ℃, standing and observing that the hydrate is completely decomposed, and putting the experimental medium in the high-pressure reaction kettle (1) into a three-phase separator (7).
3. The experiment of step 2 was repeated by changing the wax content of the white oil to 6%, 9%, 12%, 15%, respectively. And after the experiment is finished, opening the third ball valve (11), the fourth ball valve (12) and the seventh ball valve (25), separating three phases of the experiment medium, recovering the experiment medium to the water storage device (4), the oil storage device (5) and the gas storage device (6), and cleaning the high-pressure reaction kettle (1) to finish the experiment.

Claims (5)

1. The utility model provides a hydrate formation experimental apparatus under memory effect influences which characterized in that: the device comprises a high-pressure reaction kettle (1), an air supply system (2), a liquid supply system (3), a water storage device (4), an oil storage device (5), a gas storage device (6), a three-phase separator (7), a centrifugal pump (8), a first ball valve (9), a second ball valve (10), a third ball valve (11), a fourth ball valve (12), a fifth ball valve (13), a sixth ball valve (14), a first temperature transmitter (15), a second temperature transmitter (16), a pressure transmitter (17), a temperature control system (18), a magnetic stirrer (19), a flowmeter (20), a vacuum pump (21), a safety valve (22), a temperature and pressure acquisition system (23), a computer (24), a seventh ball valve (25), an eighth ball valve (26) and a ninth ball valve (27).
2. The experimental device for generating hydrates under the influence of memory effect according to claim 1, characterized in that: the high-pressure reaction kettle (1) is provided with a visual window.
3. The experimental device for generating hydrates under the influence of memory effect according to claim 1, characterized in that: the temperature and pressure acquisition system (23) acquires the pressure and temperature of the high-pressure reaction kettle (1).
4. The experimental device for generating hydrates under the influence of memory effect according to claim 1, characterized in that: the water storage device (4) is provided with a liquid injection port.
5. The experimental device for generating hydrates under the influence of memory effect according to claim 1, characterized in that: when a hydrate formation experiment is carried out under the influence of a memory effect with a history of formation of primary and secondary hydrates, the number of experiments can be reduced from n + n + n times to 1+ n + n times.
CN202011276393.0A 2020-11-16 2020-11-16 Hydrate formation experimental apparatus under influence of memory effect Pending CN112452277A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101558154A (en) * 2006-09-21 2009-10-14 维莱尼姆公司 Phospholipases, nucleic acids encoding them and methods for making and using them
US20110081729A1 (en) * 2008-01-03 2011-04-07 Baker Hughes Incorporated Hydrate Inhibition Test Loop
US20130239672A1 (en) * 2012-03-13 2013-09-19 Korea Institute Of Geoscience And Mineral Resources Apparatus for extracting, analyzing, and storing gas in drilled core on ship
CN105820857A (en) * 2016-02-26 2016-08-03 菏泽学院 Composite anti-slagging melting inhibitor used for converting low-melting point carbon-containing substances, and preparation method thereof
CN112162085A (en) * 2020-09-27 2021-01-01 西南石油大学 Experimental device for simulating influence of salinity on pore natural gas hydrate

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101558154A (en) * 2006-09-21 2009-10-14 维莱尼姆公司 Phospholipases, nucleic acids encoding them and methods for making and using them
US20110081729A1 (en) * 2008-01-03 2011-04-07 Baker Hughes Incorporated Hydrate Inhibition Test Loop
US20130239672A1 (en) * 2012-03-13 2013-09-19 Korea Institute Of Geoscience And Mineral Resources Apparatus for extracting, analyzing, and storing gas in drilled core on ship
CN105820857A (en) * 2016-02-26 2016-08-03 菏泽学院 Composite anti-slagging melting inhibitor used for converting low-melting point carbon-containing substances, and preparation method thereof
CN112162085A (en) * 2020-09-27 2021-01-01 西南石油大学 Experimental device for simulating influence of salinity on pore natural gas hydrate

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
于欢: "石墨烯/TiO2复合材料改性水性聚氨酯防污涂层研究", 《中国优秀硕士学位论文全文数据库(电子期刊)工程科技II辑》 *
田永嘉: "水合物生长赋存及记忆效应特定的实验研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 *
郑海敏: "水合物在油-气-水-蜡多相体系中诱导与生长过程研究", 《中国博士学位论文全文数据库(电子期刊)工程科技I辑》 *

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