CN110186832A - A kind of the visual exam device and analogy method of deposit structure change - Google Patents

A kind of the visual exam device and analogy method of deposit structure change Download PDF

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Publication number
CN110186832A
CN110186832A CN201910511418.1A CN201910511418A CN110186832A CN 110186832 A CN110186832 A CN 110186832A CN 201910511418 A CN201910511418 A CN 201910511418A CN 110186832 A CN110186832 A CN 110186832A
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pressure
reaction kettle
inner tube
gas
sample
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CN110186832B (en
Inventor
邱海峻
陆程
孙晓晓
陆红锋
马超
李占钊
耿澜涛
王偲
刘纪勇
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Guangzhou Marine Geological Survey
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Guangzhou Marine Geological Survey
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Priority to JP2019172979A priority patent/JP6824354B2/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/082Investigating permeability by forcing a fluid through a sample
    • G01N15/0826Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/088Investigating volume, surface area, size or distribution of pores; Porosimetry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N2015/0846Investigating permeability, pore-volume, or surface area of porous materials by use of radiation, e.g. transmitted or reflected light

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Fluid Mechanics (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The embodiment of the invention discloses a kind of visual exam devices of deposit structure change, the state adjustment system and CT scan system being connect including reaction kettle, respectively with the reaction kettle, data collection system is installed in the reaction kettle, and the data collection system passes through processor and state adjustment system feedback link;The reaction kettle includes the outer tube and inner tube for being no magnetic transparent hollow, interval is equipped between said inner tube and the outer tube, CCD camera bracket is equipped with by power zoom bar in the interval, the CT scan system includes the magnetic calibration bar that inner tube is arranged in external CT imaging device and several, and the magnetic calibration bar is provided with magnetic identification item;The present invention in the range of whole experiment process is all included in observation, and can adjust and monitor at any time during the experiment the reaction process of hydrate by integrated application CT scan and dynamic camera, accurately obtain the change procedure of hydrate under different stress.

Description

A kind of the visual exam device and analogy method of deposit structure change
Technical field
The present invention relates to geology fields, carry out more particularly to being decomposed using technical grade CT to lanthanum chloride hydrate in deposit Quantitative observation, be depressured/heat up to probe into hydrate Microstructure of Reservoirs variation in recovery process and on macroscopic properties influence can Depending on changing experimental provision and analogy method.
Background technique
China contains wide seas under its jurisdiction huge hydrate Resources Prospect.Gas hydrates are due to energy Density is high, distribution is wide, scale is big, it is shallow, superior at hiding physicochemical condition to bury, and the natural gas of output is able to satisfy the energy, economy, ring The features such as border and efficiency need is the new cleaning fuel and petroleum gas of internationally recognized most commercial exploitation prospects It is optimal to take over the energy.Carrying out gas hydrates pilot production has great strategic significance to guarantee national energy security.
South Sea hydrate preserves in without consolidation muddy siltstone reservoir, and characteristic determines during pressure reduction, Decomposition of hydrate easily leads to the sedimentation and deformation or even failure by shear of sedimentary, causes a series of engineering problems such as shaft bottom sand plug.Together When, reservoir structure variation further influences reservoir porosity and permeability properties, directly affects the production of decomposition of hydrate gas and water Out.It therefore is hydrate decompression recovery process pith for the structure change research of decomposition of hydrate process deposits.Mesh Before, it is less for the research of the structure change of hydrate shale silty sand reservoir, for more in the permeability research of hydrate reservoir Reservoir is had ignored to change in effective stress structure caused by deposit.In the reality for visual Study In Reservoir structure change Experiment device and experimental method field almost blank out.Therefore, research and development observable shale flour sand reservoir is in decomposition of hydrate process The measuring device of middle reservoir structure variation, reservoir caused by development sea area hydrate reservoir structure change that can be tentative permeate The measurement experiment of rate porosity variation, grasp under different stress conditions hydrate decomposable process Microstructure of Reservoirs change procedure with And various information such as infiltration variation characteristic.
Summary of the invention
The invention aims to provide one kind to relate to the use of technical grade CT to lanthanum chloride hydrate decomposition progress in deposit Quantitative observation, be depressured/heat up to probe into hydrate Microstructure of Reservoirs variation in recovery process and on macroscopic properties influence can Depending on changing experimental provision and visualized experiment analogy method.
Particularly, the present invention provides a kind of visual exam dress of deposit structure change during gas hydrate dissociation It sets, the state adjustment system and CT scan system connecting including reaction kettle, respectively with the reaction kettle are pacified in the reaction kettle Equipped with data collection system, and the data collection system passes through processor and state adjustment system feedback link;
The reaction kettle includes the outer tube and inner tube for being no magnetic transparent hollow, is equipped between said inner tube and the outer tube It is spaced, is provided with several equally distributed point-like support seats in the interval, pass through vibration damping silica gel between point-like support seat Pad is provided with several installation grooves around interior pipe surface, and CCD camera bracket, institute are provided in each installation groove It states and power zoom bar is installed on CCD camera bracket;
The CT scan system includes the magnetic calibration bar that inner tube is arranged in external CT imaging device and several, several Magnetic calibration bar described in root is evenly distributed on the inner wall of inner tube using the initial position of inner tube as zero point, and is located on different location The magnetic identification item of different length and different magnetic intensities is arranged according to the angle rotated from zero point for magnetic calibration bar.
In an embodiment of the invention, the outer tube both ends are respectively arranged with the upper mounting seat of built-in interface channel And lower mounting seat, the both ends of said inner tube are respectively equipped with top connection and lower contact with hollow passageway, the top connection is under Connector is correspondingly connected with respectively by the inside of the fixed outer tube of inner tube with the upper mounting seat and lower mounting seat.
In an embodiment of the invention, the upper mounting seat and lower mounting seat are respectively arranged with inserts with externally threaded Head, the outer tube are screwed on the plug by the internal screw thread at both ends, are provided with internal thread hole on the plug, it is described on connect One end of head and lower contact passes through external screw thread respectively and is screwed in the internal thread hole of the plug, the top connection and lower contact it is another One end is sealed respectively in the both ends of insertion said inner tube, and the interior tube space between the top connection and lower contact is the reaction of sample Space.
In an embodiment of the invention, the state adjustment system include gas handling system, liquid injection system, ring pressure it is cold But system and back pressure system, the gas handling system from the bottom end of the reaction kettle into the reaction kettle for the methane of specified pressure Gas, the liquid injection system inject liquid into the reaction kettle from the bottom end of the reaction kettle, and the ring pressure cooling system is used In making the response sample be maintained at the low temperature environment under specified pressure by injecting circulating frozen liquid into the reaction kettle In, while providing experiment required sample loop pressure, the back pressure system is connect with the top of the reaction kettle, for protecting in an experiment Holding system pressure, to be in any setting pressure constant.
In an embodiment of the invention, the company of the intake line of the ring pressure cooling system and the upper mounting seat Road connection is connected, freezing liquid is injected with the space between the inner wall and said inner tube to the outer tube, the upper mounting seat passes through Interface channel is connect with the output pipe of ring pressure cooling system freezing liquid is discharged.
In an embodiment of the invention, lift stand is provided on the outside of the outer tube both ends, on the lift stand It is mounted on rotation gear, the rotation gear passes through the servo motor driving being arranged in inside lift stand, in the rotary teeth Wheel side is equipped with ring rotation calibration disk, and the tooth form engaged with rotation gear is fixedly installed in the both ends end of the outer tube Turntable, the rotation gear rotates 0-360 ° in tooth form turntable, and is provided between the rotation gear and tooth form turntable Anti-rock elastic cushion.
In addition, the present invention also provides the visualized experiment moulds of deposit structure change during gas hydrate dissociation Quasi- method, includes the following steps:
Reaction kettle is added after dry as sample in step 100, the hydrate shale silty sand ground raw material for choosing corresponding area It in inner tube, is placed in CT scan system after assembling reaction kettle, then connects each auxiliary system, then acquire system by data System control experimentation;
Step 200 injects liquid by state adjustment system into reaction kettle, and adjust inner and outer tubes temperature, Ring pressure and displacement pressure gradient;
Step 300 starts sample to scan and obtain the sample under current state in dead-center position starting CT scan system Image starts the Dynamic Graph that CCD camera acts on shooting sample surfaces transformation by zoom at the same time, is scanned to the process The image of example reaction process is obtained with camera shooting;
Step 400, rotational response kettle, the different location for adjusting inner tube repeat the above steps up to the number for completing setting, After the completion of experiment, gray proces and three-dimensional reconstruction are carried out to CT image obtained in conjunction with CCD dynamic image.
In an embodiment of the invention, the specific steps of displacement are as follows:
Step 201, control liquid injection system inject liquid into inner tube from lower mounting seat, and control ring presses cooling system to outer tube Interior circulation injection freezing liquid simultaneously to provide ring pressure to inner tube cooling simultaneously, wherein the displacement pressure gradient of liquid is in inner tube 3MPa/m, and the ring pressure in outer tube keeps 0.2MPa bigger than displacement pressure;The outlet pressure of reaction kettle is atmospheric pressure;
Liquid injection system is closed after step 202, the sample water saturation in inner tube, opens gas injection system by lower mounting seat Gas is injected into inner tube, gas displacement pressure gradient is less than 3MPa/m, persistently injects by 1.5-2pv after gas flow is stablized Gas;
Step 203, after the completion of displacement, connect outlet end and the back pressure system of reaction kettle, back pressure pressure and air inlet be set Pressure is identical, while synchronous increase confining pressure, reaches predetermined gas pressure in the pore pressure of sample;
Back pressure pressure is set lower than inlet pressure 0.01MPa, while confining pressure is down to setting pressure by step 204, is continued Hydration synthesis process is carried out, and up to lanthanum chloride hydrate completion, then increases ring pressure pressure with the hydrate under simulated formation pressure Reservoir state;
Further include simulation stages of mining: in the state of to sample simulated formation pressure, back pressure pressure being set, sample two is made Pressure difference under the pressure initiation mining state at end, the hydrate in sample gradually decomposes in this process.
In an embodiment of the invention, the single-phase liquid of the liquid injection system injection is distilled water, the sample The gas injected after water saturation is methane, and the freezing liquid is anti-icing fluid, and temperature is 2 DEG C.
In an embodiment of the invention, before experiment, it is also necessary to be carried out by the gas injection system using helium Air-leakage test.
The present invention compared with the existing technology, the beneficial effect is that:
(1) visual exam device of the invention can realize CT scan using the transparent outer tube of no magnetic and inner tube, while may be used also It observes experimentation, can adjust and monitor at any time the reaction process of hydrate, accurate obtain acts in reservoir effective stress Under, during decomposition of hydrate, reservoir porosity is reduced, the change procedure that permeability reduces, and is practical productive formation hydrate Solid data are provided;
(2) one aspect of the present invention is observed that the variation of sample interior in simulation process by CT scan, so as to The accurate change procedure for obtaining reservoir under stress can obtain simultaneously in addition it can combine the dynamic of CCD camera to shoot with video-corder The intuitive change procedure of sample surfaces is obtained, the variation of sample can be more accurately held under the combination of the two image data Journey;
(3) one aspect of the present invention is using CT scan treated analog image, and still further aspect can also be using directly taking the photograph The dynamic camera of record, can be in the combination of two distinct types of image it can be observed that more accurate change procedure.
Detailed description of the invention
Fig. 1 is the experimental provision connection schematic diagram of one embodiment of the present invention;
Fig. 2 is the reaction kettle structural schematic diagram of one embodiment of the present invention;
Fig. 3 is the liquid injection system structural schematic diagram of one embodiment of the present invention;
Fig. 4 is the back pressure system structural schematic diagram of one embodiment of the present invention;
Fig. 5 is the air intake system structure schematic diagram of one embodiment of the present invention;
Fig. 6 is CT scan figure after synthesized hydrate in one embodiment of the present invention;
Fig. 7 is the pore structure figure after Fig. 6 synthesized hydrate;
Fig. 8 be another embodiment of the present invention middle decomposition of hydrate after CT scan figure;
Fig. 9 is the pore structure figure after the decomposition of hydrate in Fig. 8;
Figure 10 is the structural schematic diagram at the interval of one embodiment of the present invention;
Figure 11 is the structural schematic diagram of the lift stand of one embodiment of the present invention.
In figure: 1- reaction kettle;2- data collection system;3-CT scanning system;4- ring presses cooling system;5- gas handling system; 6- liquid injection system;The interval 7-;8- lift stand;9- back pressure system;
11- outer tube;12- inner tube 13- lower mounting seat;14- upper mounting seat;15- top connection;16- lower contact;17- pedestal;
Interface channel under 131-;The upper interface channel of 141-;
501- air compressor;502- gas booster pump;503- low pressure storage tank;504- high pressure storage tank;505- pressure regulator valve; 506- flow controller;507- gas damping device;508- cooler;
601- constant speed and constant pressure pump;602- hydraulic adjustment piston;603- four-way valve;
71- point-like support seat;72- vibration damping silicagel pad;73- installation groove;74-CCD camera support;75- power zoom bar; 76- magnetic calibration bar;77- magnetic identification item;
81- rotates gear;82- anti-rock elastic cushion;83- ring rotation demarcates disk;84- tooth form turntable;
901- back-pressure valve;902- back pressure meter A;903- back pressure meter B;904- back pressure container;905- gas-liquid separator;906- gas Tank;907- gravity measure device.
Specific embodiment
As shown in Figure 1, one embodiment of the present invention provides a kind of gas hydrate dissociation process visualization experiment dress It sets, with the decomposing state of simulating hydrate in predefined conditions, provides reference for the hydrate exploitation of actual formation.Experiment dress The state adjustment system connecting including reaction kettle 1, respectively with the reaction kettle 1 and CT scan system 3 are set, in the reaction kettle 1 Data collection system 2 is inside installed, and the data collection system 2 passes through processor and state adjustment system feedback link.Institute State state adjustment system gas handling system 5, liquid injection system 6, ring pressure cooling system 4 and back pressure system 9, the work of above-mentioned each system Process is controlled by data collection system 2.
As shown in Fig. 2, the reaction kettle 1 for containing sample and as reacting environment, mainly includes hollow 11 He of outer tube Inner tube 12, the two use sleeve structure, and outer tube 11 and inner tube 12 are made by the transparent material of no magnetic respectively, in order to observe sample Reaction process and facilitate CT scan, specific transparent material can use polyimides.Wherein, pacify respectively at the both ends of outer tube 11 Equipped with the upper mounting seat 14 and lower mounting seat 13 for having lower interface channel 131 and upper interface channel 141, lower 131 He of interface channel Upper interface channel 141 is used for gas and liquid disengaging for the input of each system, and the both ends of inner tube 12 are respectively by with hollow logical The top connection 15 and lower contact 16 in road are fixed on the inside of outer tube 11 after connecting with upper mounting seat 14 and lower mounting seat 13, after fixed Inner tube 12 and outer tube 11 inner wall between have interval.
Upper mounting seat 14 and lower mounting seat 13 are respectively arranged with the internal screw thread for passing through both ends with externally threaded plug, outer tube 11 It is screwed on the plug of upper mounting seat 14 and lower mounting seat 13 respectively, is provided centrally with tapped concave hole in plug, on One end of connector 15 and lower contact 16 passes through external screw thread respectively and is screwed in the concave hole of plug, top connection 15 and lower contact 16 it is another One end is sealed respectively in the both ends of insertion inner tube 12, and top connection 15 and lower contact 16 be inserted into after be spaced between the two away from From as the placement space of sample and reacting environment, the reacting environment need in the scanning range of CT scan system.
To improve leakproofness, it is cased in one end that inner tube 12 is inserted into top connection 15 and lower contact 16 and is sealed with 12 inner wall of inner tube Sealing ring, the sealing ring in sealing contact with the internal thread hole of upper mounting seat 14 and lower mounting seat 13 is equally cased in the other end. Equally, the sealing ring with the sealing of 11 inner wall of outer tube is also equipped on the plug of upper mounting seat 14 and lower mounting seat 13.
Upper interface channel 141 and lower interface channel 131 in upper mounting seat 14 and lower mounting seat 13 respectively include with outside The outer interface channel that gap is connected between pipe 11 and inner tube 12, and the interior interface channel being connected to internal tube are pressed such as ring and are cooled down The input terminal and output end of system 4 i.e. be connected to respectively with the outer interface channel in upper and lower mounting base 14,13, liquid injection system 6 and into Gas system 5 is then connected to interior interface channel, and the two realizes respective operation by corresponding control valve.
As shown in Figure 10, it is equipped with interval 7 between said inner tube 11 and the outer tube 12, is provided with several in the interval Equally distributed point-like support seat 71 is provided with by vibration damping silicagel pad 72 around 11 surface of inner tube between point-like support seat 71 Several installation grooves 73 are arranged in the interval 7 as previously mentioned, this is located at interval within the scanning range of CT scan system Point-like support seat 71 its effect can play the role of support, and also will not influence entirety while supporting other structures The running of device can form the support construction of a hollow out by multiple equally distributed point-like support seats 71, on the one hand not It will affect the CT scan of inner tube 11, still further aspect has the space of zoom.And the vibration damping silicagel pad 72 being arranged is then to prevent Since the vibration that external force generates has an impact photographic device in scanning process, while it is arranged in a ring can play screening The effect of light, consequently facilitating the focusing of photographic device and the clarity shot with video-corder.
It is provided with CCD camera bracket 74 in each installation groove 73, is equipped on the CCD camera bracket 74 Power zoom bar 75, the CCD camera bracket 74 of setting is easy for the camera devices such as installation CCD camera, excellent in the present embodiment CCD camera is selected, certain other cameras that can satisfy resolution ratio are also possible, and in the present embodiment in order to guarantee most Good shoots with video-corder effect, is also provided with power zoom bar 75, and the effect of the power zoom bar 75 is through automatically controlled flexible mode The focal length of camera mounted thereto is controlled, to meet shoots with video-corder demand under different conditions.
In summary content, in the present embodiment, concrete mode are the sights for comprehensively considering CT scan to interior change It examines, while also capturing the outer surface variation of cleaning by external photographic device, it can be more intuitive by both modes Change procedure of the acquisition sample under stress.And in the present invention, by being arranged, multiple groups relative position is different to be taken the photograph As device, surface modified-image of the sample in different location when can capture different conditions simultaneously, due to obtaining inside CT inverted image, this comprehensive two-part content can intuitively obtain the three dimensional change process of sample.
In addition, also needing further to consider the problems of the section CT in the present invention, in the CT image that the same position obtains It is a section, it can only characterize the change procedure on a direction, and for its three-dimensional variation, there is also certain Defect, therefore in order to obtain the scanning result of multiple angles, it is also necessary in the physical location of the process transformation sample of scanning.
Before converting specific position, it is necessary first to orderly calibration is carried out to the position of sample, it is corresponding in order to reach Calibration, in the present embodiment, the CT scan system 3 include two parts, if respectively external CT imaging device and The magnetic calibration bar 76 of inner tube 11 is arranged in dry root,
Wherein using the initial position of inner tube 11 as zero point, several magnetic calibration bars 76 are evenly distributed on inner tube 11 Inner wall, and the magnetic calibration bar 76 being located on different location is according to the angle setting different length rotated from zero point and different magnetism The magnetic identification item 77 of intensity.
Herein it should be noted that in the same embodiment, the angle with zero point rotation is equal, and in difference Embodiment in, the angle be it is variable, corresponding angle can be set according to the actual demand of different samples, angle Setting is determined according to the test result of sample test.
It is distinguished with the prior art, is not only to distinguish by simple mark post in the present invention, this is because Common mark post only plays the role of calibration during the test, is no any mark in the scan image of generation 's.Therefore, in the present embodiment, distinguished by the magnetic identification item of setting different length and magnetic intensity, a side Face can have intuitive difference during test, and still further aspect is then by the structure of magnetic interference CT scan, by it Mark is shown on CT scan image, so as to the comparison and processing in later period.
As shown in figure 11, it is provided with lift stand 8 on the outside of 12 both ends of outer tube, is mounted on rotation on the lift stand 8 Rotating disk 81, the rotation gear 81 passes through the servo motor driving being arranged in inside lift stand 8, in 81 side of rotation gear Face is equipped with ring rotation calibration disk 83, and the tooth engaged with rotation gear 81 is fixedly installed in the both ends end of the outer tube 12 Shape turntable 84, the rotation gear 81 rotate 0-360 ° in tooth form turntable 84, and in the rotation gear 81 and tooth form turntable Anti-rock elastic cushion 82 is provided between 84.
In the present invention, it is to realize what angle adjusted by the engagement between servo motor and gear, changes kind of an expression and turn Control of the dynamic angle by servo motor, and the power of servo-electric is nibbled to guarantee the stabilization in transmittance process with gear The mode of conjunction is driven, in addition, influencing the effect of camera shooting to reduce vibration, also passes through the cushion of elasticity in the present invention To fill the gap between gear engagement.
Specifically, liquid injection system 6, gas handling system 5 are connect with the interface channel being connected in lower mounting seat 13 with inner tube 11, ring Cooling system 4 is pressed to connect with the interface channel that gap is connected between outer tube 11 and inner tube 12 in lower mounting seat 13, upper mounting seat 14 It connects, the interface channel that ring presses system 9 that gas-liquid is discharged with inner tube 12 in upper mounting seat 14 is connect.
Gas handling system 5, liquid injection system 6, back pressure system 9, ring pressure cooling system 4 and CT scan in the present embodiment Existing equipment in the prior art can be used in system 3, is illustrated separately below.
The connection structure of liquid injection system 6 is as shown in figure 3, the constant speed and constant pressure pump 601 of liquid injection system 6 uses HAS-200HSB type Twin-tub constant speed and constant pressure pump, quantitatively injects for displacing medium, provides power source for test.Its operating pressure is 50MPa, flow velocity There is 0.01~20mL/min pressure protection and position bound to protect, and pump head material uses 316L, which configures communication port, It can be connect with data collection system 2, two cylinder can realize that independently operation and twin-tub linkage are made for single cylinder independently working, twin-tub Industry.Specifically using distilled water or kerosene as driving medium output, the constant pressure to driving medium, constant current are realized during output It is controlled with tracking PLC.Two hydraulic adjustment pistons 602 have been installed in parallel between twin-tub constant speed and constant pressure pump 601 and lower mounting seat, Four-way valve 603, the both exportable gas-liquids, while also side of four-way valve 603 are separately installed at the both ends of each hydraulic adjustment piston 602 Just other pipelines are accessed, pipeline is such as cleaned.The volume of hydraulic adjustment piston 602 is 2000mL, operating pressure 50MPa, and material is 316L.Isolation and energy storage buffer and transmission of the hydraulic adjustment piston 602 as injection liquid and displacing fluid.It is done in cylinder inner surface flat Sliding processing, to reduce inner wall frictional force.
As shown in Figure 4.Back pressure system 9 includes the back-pressure valve 901 being connected on the pipeline of the output hydrate of upper mounting seat 14, Show the back pressure meter A902 of pressure on back-pressure valve 901, pressure is when reaction kettle output pressure exceeds standard at adjusting back-pressure valve 901 Self-relieving backpressure pump B903 and back pressure container 904 carry out the gas-liquid separator 905 of gas-liquid separation to received hydrate, Gas and the gas tank 906 measured after separating are received, the gravity measure device 907 of liquid after separation is weighed.
As shown in figure 5, gas handling system 5 injects gas into inner tube 12 by gas compressor with synthesized hydrate or measurement Gas permeability of the hydrate reservoir in different mining states.Such as pass through the injection single-phase methane gas of isothermal and precise measurement outlet Gas flow, and can measure gas permeability according to Darcy's law.
Gas handling system 5 include generate pressed gas air compressor 501, to air compressor 501 generate gas into The gas booster pump 502 of row pressurization, the low pressure storage tank 503 of low-pressure gas after storage pressurization, the height of high pressure gas after storage pressurization Storage tank 504 is pressed, inputs the pressure regulation of specified pressure into inner tube according to requirement of experiment selection low pressure storage tank 503 or high pressure storage tank 504 Valve 505, and the flow controller 506 of control output gas flow of gas size, the cooler 508 of cooling gas and liquid;In pressure regulation Gas damping device 507 is installed in the gas circuit before valve 505, which is the pressure vessel equipped with liquid, Make by gas soak naturally.
Cooler 508 is for the gas and liquid in cooling injection reaction kettle, and gas and liquid is not after cooling treatment Destruction can be generated to the hydrate equilibrium state in reaction kettle.The product of model GCS50 can be selected in air compressor 501, Design pressure is 1.0MPa, flow 0.465m3/min, and the cleaning that air compressor 501 can also be used in entire pipe-line system is swept Gas.SITEC type gas-gas inflator, model GBD60, pressure ratio 60:1, maximum outlet pressure can be selected in the gas booster pump 502 498Bar, maximum stream flow 40L/min.Low pressure storage tank 503 is mainly used for storing the pressurized air of air compressor 501, needs Meet following condition: volume 0.1m3, operating pressure 0.8MPa, design pressure 1MPa.High pressure storage tank 502 needs to meet as follows: holding Product 2000mL, maximum working pressure (MWP) 50MPa.Pressure regulator valve 505 is in addition to including manual pressure regulating valve, there are also corresponding pressure indicator, It is mainly used for pressurized high pressure gas being adjusted to required operating pressure.Wherein manual pressure regulating valve maximum inlet pressure is 50MPa, outlet pressure are adjustable between 0~40MPa.Flow controller 506 uses Blang gram high-pressure flowmeter, maximum functional Pressure is 40MPa, band communication interface, can realize communication connection with data collection system 2.
Data collection system 2 includes the control system with data processing software, and control system can be PC machine, industrial personal computer Equipment etc. having data processing and analytic function.Control system controls experimentation by data processing software, while to CT Scanning system 3 and experimentation realize image and data acquisition, analysis and result output etc..
CT scan system is for accommodating the reaction kettle, to scan the variation of the sample in reaction kettle during the reaction; Specific CT instrument is the multi-scale rock 3-D scanning imaging system (open Microfocus X-ray X-ray scanning) of three English companies production.
At work, the inner tube 11 and outer tube 12 of mounted reaction kettle 1, while each system is connected, to inner tube 12 A main line connection can be used in fluid injection, water filling, gas injection, and then each system is connected using being in charge of with control valve with supervisor, Corresponding control valve is opened when needing.Reaction kettle 1 is placed in the scanning room of CT scan system 3, is needing x-ray scanning source just To the space for accommodating sample between upper and lower connector 14,13.Wherein, gas handling system 5 provides the methane of specified pressure to reaction kettle 1 Gas;Liquid injection system 6 provides water for the sample in reaction kettle 1;Ring pressure cooling system 4 injects circulating frozen liquid into reaction kettle 1 Be maintained at response sample in the low temperature environment under specified pressure;Back pressure system 9 is connect with the top of reaction kettle 1, is used for Keep the pressure on top identical as the pressure of bottom end after completing experiment;And CT scan system 3 is being tested for scanning response sample The modified-image of process;Data collection system 2 controls the work of each system according to requirement of experiment, and acquires in experimentation Various data are analyzed and are exported.It is described in detail in the description of specific course of work method below.
Present embodiment can realize CT scan using the transparent outer tube of no magnetic and inner tube, while also can be observed to test Journey can adjust and monitor at any time the reaction process of hydrate, accurate to obtain under the effect of reservoir effective stress, decomposition of hydrate In the process, reservoir porosity reduces, and the change procedure that permeability reduces provides solid for practical productive formation hydrate Data.
In an embodiment of the invention, a kind of aforementioned gas hydrate dissociation process visualization experiment dress is disclosed The application method set, generally comprises the steps:
Step 100, the hydrate shale silty sand ground raw material of corresponding area is chosen as sample, and reaction kettle is added after dry It in inner tube, is placed in CT scan system after assembling reaction kettle, then connects each auxiliary system, then acquire system by data System control experimentation;
Sample drying can be realized by barbecue or drying box.Here auxiliary system refers to the gas handling system 5 of front, note Liquid system 6, ring pressure cooling system 4 and back pressure system 9.Reaction kettle 1 after making installation for convenience keeps stablizing, can be in reaction kettle A cup dolly 17 is arranged in 1 bottom, and reaction kettle 1 is fixed on the center point of pedestal 17 by lower mounting seat 13, then the bottom of by Seat 17 is placed on together on the mounting table of CT scan system 3 together with reaction kettle 1, and pedestal 17 forms fixation by screw and mounting table Connection.
Before experiment, gas handling system 5 is first passed through to the test of being sealed property of helium is injected in reaction kettle 1 in advance, with determination The accuracy and safety of experiment.
It is adjusted using X-ray of the data collection system 2 to CT scan system 3, meets it at a distance from reaction kettle 1 Scanning requires.
Step 200, control liquid injection system injects liquid into inner tube from lower mounting seat, and control ring presses cooling system to outer tube Interior circulation injection freezing liquid simultaneously to provide ring pressure to inner tube cooling simultaneously, wherein the displacement pressure gradient of liquid is in inner tube 3MPa/m, and the ring pressure in outer tube keeps 0.2MPa bigger than displacement pressure;The outlet pressure of reaction kettle is atmospheric pressure;
The injection rate of liquid needs that the internal sample filled is made to reach saturated-water phase, and the liquid injected here is single-phase liquid Body, specially distilled water;It determines whether water injection rate meets the requirements, the upper mounting seat 14 and inner tube 12 of observing response kettle 1 can be passed through Whether the interface channel of connection is discharged water, shows that inside is in a saturated state when water is discharged, can continue to infuse after water outlet Enter distilled water 1.5-2PV, then stops the work of liquid injection system 6.The freezing liquid that ring pressure cooling system 4 uses is anti-icing fluid, temperature It is 2 DEG C.
Step 300, liquid injection system is closed after the sample water saturation in inner tube, opens gas injection system by lower mounting seat Gas is injected into inner tube, gas displacement pressure gradient is less than 3MPa/m, persistently injects by 1.5-2pv after gas flow is stablized Gas;
Here the gas injected is methane, and the pressure at 12 upper end outlet of inner tube is atmospheric pressure at this time.To gas flow rate It can continue to inject 1.5-2pv gas after stabilization.
Step 400, after the completion of displacement, outlet end and the back pressure system of reaction kettle are connected, back pressure pressure and air inlet are set Pressure is identical, while synchronous increase confining pressure starts CT scan system pair when the pore pressure of sample reaches predetermined gas pressure Sample starts to scan and obtain the sample image under current state;
The pore pressure of sample can be gradually increased after lasting air inlet, confining pressure pressure needs consistently greater than pore pressure 0.2MPa.When CT scan, need to keep gas pressure and confined pressure steady.
Step 500, back pressure pressure is then set lower than inlet pressure 0.01MPa, while confining pressure is down to setting pressure, Hydration synthesis process is persistently carried out, and up to lanthanum chloride hydrate completion, then increases ring pressure pressure with the water under simulated formation pressure Object reservoir state is closed, and the process is scanned to obtain the image of example reaction process;
Step 600, after the completion of experiment, gray proces and three-dimensional reconstruction is carried out to CT image obtained, can be obtained and set Under fixed condition when productive formation hydrate, the decomposing state and reservoir structure of hydrate change.
Present embodiment carries out lanthanum chloride hydrate under 1MPa effective stress and decomposes real for shale silty sand reservoir samples It tests, experimental result is shown under the effect of reservoir effective stress, and with decomposition of hydrate, reservoir porosity is reduced, and permeability reduces. For shale silty sand reservoir, when wherein decomposition of hydrate, there are two kinds of effects: 1, decomposition of hydrate reservoir pore space increases hole Porosity increases;2, reservoir pressure reduces decomposition of hydrate, and reservoir effective stress is caused to increase, and reservoir pore space is empty under compression Between reduce.Experimental result, which is shown under two kinds of effects, eventually leads to reservoir porosity reduction, and permeability lowers, illustrates for shale Silty sand reservoir, stratum effective stress plays a leading role in reservoir porosity and permeability variation during decomposition of hydrate.
In an embodiment of the invention, simulation stages of mining can also be increased: to sample simulated formation pressure Under state, back pressure pressure is set, the pressure difference under the pressure initiation mining state at sample both ends is made, being obtained using CT scan system should Decomposition of hydrate image in sample in the process.
Following specific embodiments explanation, the use process of this experimental provision.
1. shale silty sand sample is taken, it is 12 hours dry in drying box.It takes out sample and is broken into that diameter is 2mm or so Grain.6g sample is taken to be fitted into reaction kettle inner cavity.
2, cryogenic high pressure system is assembled.Reaction kettle is fixed on the objective table of focal spot x-ray CT instrument by pedestal, is connected The pipeline of gas injection system and the confining pressure circulatory system.It is tested using leakproofness of the helium to system.
3, gas injection system valve V1 is closed, liquid injection system valve V2 and confining pressure cooling recirculation system are opened, is arranged cold Circulating temperature is 2 DEG C, closes gas back pressure system valve V4, opens reaction kettle outlet valve V3, outlet pressures are atmosphere Pressure.The pressure that liquid injection is arranged is 0.7MPa.Setting confining pressure system pressure is 0.6MPa.Liquid infusion pump is opened, list is used Phase liquid (distilled water) saturated sample.Continue to inject distilled water 1.5-2PV after the water breakthrough of outlet end.
4, the valve V2 of liquid injection system is closed.It is connected to liquid injection system and reaction kettle.Using 0.7MPa methane gas to reaction Saturation water sample carries out displacement test in kettle.Inlet port is measured by gas flowmeter, is stablized to fluid flow rate subsequent Continuous injection 1.5-2pv gas.
5, after the completion of displacement, valve V3 is closed, valve V4 is opened, reaction kettle outlet end is connect with back pressure system.Setting Back pressure pressure is identical as admission pressure.Gas pressure continues gas injection before holding, and is gradually increased sample pore pressure, while same Step increases confining pressure, and confining pressure pressure is kept to be greater than pore pressure 0.2MPa.Pore pressure is increased into 8MPa, confining pressure pressure is 8.2MPa.Maintain gas pressure and confined pressure steady.X-ray CT scan is carried out at this time.
6,7.98MPa circulation fluid is set by back pressure after the completion of CT scan to be depressured, keep air inlet open, persistently give Reaction kettle gas supply, enters gas constantly in reaction kettle.The pressure of ring pressure circulation is reduced to pressure is set, is hydrated Object compound experiment.
7, this state is maintained 12 hours, until lanthanum chloride hydrate is completed.
8, after the completion of scanning, increase confining pressure circulatory system pressure to 9MPa, 1MPa strata pressure situation can be simulated at this time Under hydrate reservoir state.Then CT scan and three-dimensionalreconstruction are carried out.As a result as shown in Figures 6 and 7.
9, simulation decompression recovery process.Gas feed valve is closed, is 2MPa by setting back pressure pressure, while by confining pressure pressure Power, which is arranged to 3MPa, decomposes methane in reaction kettle.CT scan is carried out to reservoir after the completion of decomposition, resulting CT image is carried out Gray proces and three-dimensional reconstruction observe hydrate decomposing state and reservoir structure variation.As a result as shown in FIG. 8 and 9.
So far, although those skilled in the art will appreciate that present invention has been shown and described in detail herein multiple shows Example property embodiment still without departing from the spirit and scope of the present invention, still can according to the present disclosure directly Determine or deduce out many other variations or modifications consistent with the principles of the invention.Therefore, the scope of the present invention is understood that and recognizes It is set to and covers all such other variations or modifications.

Claims (10)

1. a kind of visual exam device of deposit structure change, which is characterized in that including reaction kettle, respectively with the reaction kettle The state adjustment system and CT scan system of connection, are equipped with data collection system, and the data are adopted in the reaction kettle Collecting system passes through processor and state adjustment system feedback link;
The reaction kettle includes the outer tube and inner tube for being no magnetic transparent hollow, between being equipped between said inner tube and the outer tube Every, several equally distributed point-like support seats are provided in the interval, between point-like support seat pass through vibration damping silicagel pad Interior pipe surface is provided with several installation grooves, CCD camera bracket is provided in each installation groove, it is described Power zoom bar is installed on CCD camera bracket;
The CT scan system includes the magnetic calibration bar that inner tube is arranged in external CT imaging device and several, several institutes State the inner wall that magnetic calibration bar is evenly distributed on inner tube using the initial position of inner tube as zero point, and the magnetism being located on different location The magnetic identification item of different length and different magnetic intensities is arranged according to the angle rotated from zero point for calibrating stem.
2. visual exam device according to claim 1, which is characterized in that the outer tube both ends are respectively arranged with built-in connect The upper mounting seat and lower mounting seat in road are connected, the both ends of said inner tube are respectively equipped with the top connection with hollow passageway and connect under Head, the top connection and lower contact are correspondingly connected with respectively by the fixed outer tube of inner tube with the upper mounting seat and lower mounting seat It is internal.
3. visual exam device according to claim 2, which is characterized in that the upper mounting seat and lower mounting seat are set respectively It is equipped with externally threaded plug, the outer tube is screwed on the plug by the internal screw thread at both ends, is provided on the plug One end of internal thread hole, the top connection and lower contact passes through external screw thread respectively and is screwed in the internal thread hole of the plug, described The other end of top connection and lower contact is sealed respectively in the both ends of insertion said inner tube, interior between the top connection and lower contact Tube space is the reaction compartment of sample.
4. visual exam device according to claim 1, which is characterized in that the state adjustment system includes air inlet system System, liquid injection system, ring pressure cooling system and back pressure system, the gas handling system is from the bottom end of the reaction kettle to the reaction kettle The interior methane gas for specified pressure, the liquid injection system inject liquid into the reaction kettle from the bottom end of the reaction kettle, The ring pressure cooling system is used to make the response sample be maintained at finger by injecting circulating frozen liquid into the reaction kettle In low temperature environment under constant-pressure, while providing experiment required sample loop pressure, the top of the back pressure system and the reaction kettle Connection, it is constant for keeping system pressure to be in any setting pressure in an experiment.
5. visual exam device according to claim 4, which is characterized in that the intake line of ring pressure cooling system with The interface channel of the upper mounting seat connects, and injects freezing liquid with the space between the inner wall and said inner tube to the outer tube, The upper mounting seat presses the output pipe of cooling system to connect so that freezing liquid is discharged by interface channel with the ring.
6. visual exam device according to claim 1, which is characterized in that be provided with and lift on the outside of the outer tube both ends Frame, rotation gear is mounted on the lift stand, and the rotation gear passes through the servo motor being arranged in inside lift stand and drives It is dynamic, ring rotation calibration disk is installed in the rotary teeth wheel side, is fixedly installed with and revolves in the both ends end of the outer tube The tooth form turntable of rotating disk engagement, the rotation gear rotate 0-360 ° in tooth form turntable, and in the rotation gear and tooth Anti-rock elastic cushion is provided between shape turntable.
7. a kind of visualized experiment analogy method of deposit structure change, which comprises the steps of:
The inner tube of reaction kettle is added as sample in step 100, the hydrate shale silty sand ground raw material for choosing corresponding area after dry In, it is placed in CT scan system after assembling reaction kettle, then connects each auxiliary system, then pass through data collection system control Experimentation processed;
Step 200 injects liquid by state adjustment system into reaction kettle, and adjusts the temperature of inner and outer tubes, ring pressure And displacement pressure gradient;
Step 300 starts sample to scan and obtain the sample image under current state in dead-center position starting CT scan system, Starting CCD camera acts on the Dynamic Graph of shooting sample surfaces transformation by zoom at the same time, which is scanned and is taken the photograph As the image to obtain example reaction process;
Step 400, rotational response kettle, the different location for adjusting inner tube repeats the above steps until the number that completion is set, experiment After the completion, gray proces and three-dimensional reconstruction are carried out to CT image obtained in conjunction with CCD dynamic image.
8. visualized experiment analogy method according to claim 7, which is characterized in that
The specific steps of displacement are as follows:
Step 201, control liquid injection system inject liquid into inner tube from lower mounting seat, and control ring pressure cooling system is followed into outer tube Ring injects freezing liquid simultaneously to provide ring pressure simultaneously to inner tube cooling, wherein and the displacement pressure gradient of liquid is 3MPa/m in inner tube, And the ring pressure in outer tube keeps 0.2MPa bigger than displacement pressure;The outlet pressure of reaction kettle is atmospheric pressure;
Liquid injection system is closed after step 202, the sample water saturation in inner tube, and it is inside by lower mounting seat to open gas injection system Gas is injected in pipe, gas displacement pressure gradient is less than 3MPa/m, persistently injects gas by 1.5-2pv after gas flow is stablized Body;
Step 203, after the completion of displacement, connect outlet end and the back pressure system of reaction kettle, back pressure pressure and admission pressure be set It is identical, while synchronous increase confining pressure, reach predetermined gas pressure in the pore pressure of sample;
Back pressure pressure is set lower than inlet pressure 0.01MPa, while confining pressure is down to setting pressure by step 204, lasting to carry out It is hydrated synthesis process, and up to lanthanum chloride hydrate completion, then increases ring pressure pressure with the hydrate reservoir under simulated formation pressure State;
Further include simulation stages of mining: in the state of to sample simulated formation pressure, back pressure pressure being set, sample both ends are made Pressure difference under pressure initiation mining state, the hydrate in sample gradually decomposes in this process.
9. visualized experiment analogy method according to claim 7, which is characterized in that the liquid injection system injects single-phase Liquid is distilled water, and the gas injected after the sample water saturation is methane, and the freezing liquid is anti-icing fluid, and temperature is 2 DEG C.
10. visualized experiment analogy method according to claim 7, which is characterized in that before experiment, it is also necessary to pass through institute It states gas injection system and carries out air-leakage test using helium.
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