CN106872497A - The special hydrate resistivity test devices of CT and method - Google Patents
The special hydrate resistivity test devices of CT and method Download PDFInfo
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- CN106872497A CN106872497A CN201710303350.9A CN201710303350A CN106872497A CN 106872497 A CN106872497 A CN 106872497A CN 201710303350 A CN201710303350 A CN 201710303350A CN 106872497 A CN106872497 A CN 106872497A
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- 238000012360 testing method Methods 0.000 title claims abstract description 18
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- 230000035515 penetration Effects 0.000 claims abstract description 44
- 238000005259 measurement Methods 0.000 claims abstract description 41
- 238000005520 cutting process Methods 0.000 claims abstract description 20
- 230000008569 process Effects 0.000 claims abstract description 17
- 239000013049 sediment Substances 0.000 claims abstract description 17
- 238000013170 computed tomography imaging Methods 0.000 claims abstract description 16
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- 239000004696 Poly ether ether ketone Substances 0.000 claims abstract description 6
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920002530 polyetherether ketone Polymers 0.000 claims abstract description 6
- 238000002347 injection Methods 0.000 claims description 24
- 239000007924 injection Substances 0.000 claims description 24
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- 238000006073 displacement reaction Methods 0.000 claims description 15
- 229910000831 Steel Inorganic materials 0.000 claims description 11
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- 238000009826 distribution Methods 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 6
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 claims description 5
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- 238000007789 sealing Methods 0.000 description 10
- 238000000151 deposition Methods 0.000 description 7
- NUXZAAJDCYMILL-UHFFFAOYSA-K trichlorolanthanum;hydrate Chemical compound O.Cl[La](Cl)Cl NUXZAAJDCYMILL-UHFFFAOYSA-K 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
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Abstract
The present invention relates to the special hydrate resistivity test devices of CT and method, described device includes ray penetration clamper, resistivity measurement module, confined pressure control module, temperature control module, pore pressure control module, data acquisition module and CT imaging systems；Ray penetration clamper includes pressure-bearing pipe, end cover, cutting ferrule nut, and pressure-bearing pipe uses PEEK materials；Pore pressure fluid issuing and confined pressure fluid issuing are provided with upper end cover, pore pressure fluid intake and confined pressure fluid intake are provided with bottom end cover；Including resistivity probe, resistivity probe casing and annular electrode etc., annular electrode is set in qually spaced on resistivity probe resistivity measurement module.By the device both can Accurate Determining hydrate generate decomposable process in resistivity Spatial Variation, can realize again X CT scan be imaged, so as to realize the synchro measure of hydrate sediment system resistivity and pore communication temporal and spatial evolution.
Description
Technical field
The invention belongs to the physical parameter such as ocean gas hydrate reservoir resistivity e measurement technology and application field, specifically
It is related to a kind of hydrate resistivity test device and method for X-CT detections.
Background technology
Gas hydrates are widespread in nature, and are mainly distributed on the ocean shelf margin below 300 meters of the depth of water
Or dirt band area, it is considered to be a kind of potential energy resources.The conductive capability of different materials is also not to the utmost in nature
It is identical, and conductive capability can be represented with electrical parameters such as impedance, resistivity.In bottom sediment due to preservation gas water
There is obvious change in compound, its resistance characteristic, therefore, electrology characteristic is the main physical parameter of hydrate reservoir.By surveying
Change in resistance in amount bottom sediment stratum, you can judge hydrate reservoir, is further satisfied by resistivity and hydrate
With the quantitative analysis of degree, the reserves of gas hydrates are can be evaluated whether.
At present, existing laboratory hydrate resistivity measurement technology is all based on macro-scale both at home and abroad, using difference
Electrode or sensor, to sediment in high-voltage penetration clamper or different layers position test, the result is that
Whole system or certain layer of average resistance change of position, because gas hydrates generation is random, it is in deposit hole
In it is pockety, therefore be currently based on macroscopic resistance rate detection experimental result can not accurately portray hydrate storage shape
State and its influence of the distribution situation to resistivity in deposit hole；Deposit inside hydrate micro Distribution cannot be reflected
Influence of the condition to resistivity, cannot especially judge change in resistance rule and deposition in lanthanum chloride hydrate or generating process
The response pattern of thing pore throat Parameters variation, it is impossible to explain change in resistance in hydrate generation, decomposable process from micro-scale
Mechanism.
In fact, during gas hydrates are generated or are decomposed, the dissolving in deposit pore communication, hole
Gas, water and ion concentration can all change, and these exactly change the principal element of reaction medium electric conductivity.In hydration
Sediment microstructure detection aspect, also there is the research of correlation the country：As publication number CN102636503B discloses a kind of day
The right gas hydrate special ray penetration clamper of natural core CT reformations and method；Publication number CN101246117B and
It is micro- with CT that the patent of invention of CN104155188B will contain hydrate sediment mechanics parameter measurement apparatus from different angles respectively
See Detection Techniques to combine, invent the method that deposit change of mechanical property rule is explored in grand microcosmic combination.
But there is no shout what structure detection was combined with the microcosmic hole containing hydrate sediment specifically designed for resistance parameter at present
Experimental provision or method, it is difficult to the parameters such as the dissolved gas in hydrate concentration, deposit pore communication, hole and electricity
Dependency relation between resistance rate score carries out quantitative analysis.Therefore, develop it is a set of i.e. both can Accurate Determining hydrate generation decomposed
Resistivity in journey, can simultaneously observe the experiment of the situation of change of deposit pore communication, hydrate, dissolved gas and water again
Test device and method, to obtaining reliable resistivity with hydrate concentration dependency relation, the stock number estimation of raising hydrate
The degree of accuracy it is significant, it helps the resistance parameter change rule from lanthanum chloride hydrate and decomposable process is explained in mechanism
The microcosmic response mechanism of rule.
The content of the invention
The technical problems to be solved by the invention are in view of the foregoing defects the prior art has, there is provided a kind of CT is special
Hydrate resistivity test device and method, described device are placed on the transmission imaging turntable of X-CT imaging systems, both can be accurate
The resistivity in hydrate generation decomposable process is really determined, X-CT scanning imageries can be simultaneously realized again, so as to observe deposit hole
The situation of change of gap connectedness, hydrate, dissolved gas and water, realizes hydrate sediment system resistivity and porosity communication
The synchro measure of property.
The present invention is realized using following technical scheme：The special hydrate resistivity test devices of CT, including ray
Penetration clamper, resistivity measurement module, confined pressure control module, temperature control module, pore pressure control module, data acquisition module with
And it is arranged on the CT imaging systems of ray penetration clamper both sides；The temperature control module, confined pressure control module and pore pressure control
Molding block is connected with ray penetration clamper；The data acquisition module is imaged system with resistivity measurement module and CT respectively
System is connected；
The ray penetration clamper includes pressure-bearing pipe, end cover, cutting ferrule nut, and pressure-bearing pipe uses PEEK materials,
Wall thickness is less than 2mm, and the inside of pressure-bearing pipe is provided with deposit sample glue bucket, and the two ends of deposit sample glue bucket are provided with die sleeve slug；
The two ends lateral wall of pressure-bearing pipe is provided with cutting ferrule fixed lobe, the cutting ferrule fixed lobe and cutting ferrule nut screw connection, by sealed end
Lid is fixed with pressure-bearing pipe；The end cover includes being separately positioned on the upper end cover and bottom end cover at pressure-bearing pipe two ends, described
Pore pressure fluid issuing and confined pressure fluid issuing are provided with upper end cover, are respectively arranged with bottom end cover and pore pressure control module and enclosed
Pressure control module connected pore pressure fluid intake and confined pressure fluid intake, and be provided with pore pressure fluid issuing and deposit sample
The pore pressure outflow pipeline of glue bucket connection；
The resistivity measurement module includes combined type multi-point resistivity probe and resistivity monitoring switching device, with
The resistivity data of sample under acquisition different condition；The combined type multi-point resistivity probe includes resistivity probe, resistance
Rate probe casing and annular electrode, the annular electrode are set in qually spaced on resistivity probe, and the resistivity probe passes through
Pore pressure outflow pipeline is inserted into inside deposit sample.
Further, the confined pressure control module includes the plunger displacement pump confined pressure circulatory system and Back pressure control valve, and plunger displacement pump encloses
The pressure circulatory system is connected by Back pressure control valve with confined pressure fluid outlet, and pressure is provided using the plunger displacement pump confined pressure circulatory system
Source, coordinates Back pressure control valve to realize that system confined pressure is controlled, and confined pressure maximum 10Mpa, Back pressure control valve is automatically controlled by a computer, can
To set the height of confined pressure and automatically control, confined pressure control accuracy reaches 0.1FS.
Further, the temperature control module includes constant temperature air bath control cabinet and circulating temperature control system, loop temperature-control system
Injection pipeline with the plunger displacement pump confined pressure circulatory system is connected, and for controlling the temperature in fluid circuit, clamps ray penetration
Can be realized at device import by temperature control between -5 DEG C-room temperature, under both collective effects, realize temperature-controlled precision ±
0.5℃。
Further, the pore pressure control module includes plunger pump priming system, steel cylinder gas injection system and pressure reduction control valve,
The steel cylinder gas injection system is connected by pressure reduction control valve with plunger pump priming system, is then commonly connected to pore pressure fluid intake
End, plunger pump priming system mixes injection with steel cylinder gas injection system before ray penetration clamper pore pressure fluid intake, and leads to
Cross the pressure balance of both pressure reduction control valve control, it is to avoid gas pours into plunger pump priming system or liquid enters steel cylinder gas injection system
System.
Further, actually active length of the resistivity probe in deposit sample is inserted into is 40mm, described
Annular electrode includes 4, and the distance between adjacent annular electrode is 10mm, and each annular electrode both can be as electron emission
Pole, it is also possible to as electronic receipt pole, can thus measure deposit internal resistance rate value and amount toGroup, effectively observation
The Spatial Variation of resistivity in lanthanum chloride hydrate and decomposable process.
Further, the external diameter of the resistivity probe casing is 3mm, using hard insulation, resistance probe sleeve pipe
With the annular space between pore pressure outflow pipeline for actual apertures hydraulic fluid flow goes out passage.
Further, seal convexity at two, die sleeve slug and deposit sample glue bucket are provided with the die sleeve slug
Between interference fit, seal deposit sample, to further enhance deposit sample two ends sealing, prevent pore pressure, confined pressure from ganging up.
Further, O-ring seal mounting groove is provided between the pressure-bearing pipe madial wall and end cover, by O-shaped
Circle installs the sealing that the sealing ring of inside grooves is realized between end cover and pressure-bearing pipe.
Further, described pore pressure fluid intake, pore pressure fluid issuing are arranged at the center of end cover, and point
Be not connected with die sleeve slug by pore pressure fluid inlet line and pore pressure fluid issuing pipeline, realize pore pressure injection and
Output.
Further, to prevent the fixing nut between pore pressure fluid issuing and confined pressure fluid issuing from interfering,
And preventing pore pressure fluid intake and confined pressure fluid intake from interfering, the confined pressure fluid issuing is internally provided with upper end cover
To the hole that end cover outer rim flows, and confined pressure fluid intake is internally provided with the hole flowed to bottom end cover outer rim in bottom end cover
Gap, convenient experiment.
The present invention is also disclosed a kind of measuring method using the special hydrate resistivity test devices of above-mentioned CT in addition, including
Following steps：
(1) dress sample and installation：
1. ray penetration clamper is opened, deposit is filled up in deposit sample glue bucket and is added the appropriate aqueous solution；
2. resistivity probe casing and resistivity probe, end cover are inserted；
3. ray penetration clamper is installed on CT imaging system objective tables；
(2) gas hydrates are generated：
1. temperature control module switch is opened, circulating water temperature is set, make sediment sample temperature in ray penetration clamper
Reach the temperature requirements of experiment；
2. setting liquid is injected to sample interior to setting pressure by piston pump liquid injection system；Regulation pressure reduction control valve,
Add reacting gas so that the pressure needed for pressure reaches experiment in ray penetration clamper；
3. pressure source is provided using the plunger displacement pump confined pressure circulatory system, coordinates Back pressure control valve, needed for realizing system experimentation
System confined pressure；Because there is provided suitable temperature, pressure condition, gas hydrates start generation, and are progressively filled into deposition
In thing hole；
(3) gas hydrate dissociation is simulated：
1. after step (2) is fully finished, temperature control module continuous firing is kept；Pore pressure inlet valve is closed, is progressively opened
The valve of pore pressure fluid issuing, simulating hydrate step-down decomposable process；Or
2. pore pressure fluid inlet valve is closed, is gradually heated up to system by temperature control module, and by controlling pore pressure fluid
Outlet valve realizes that the pressure inside ray penetration clamper is in steady state, the intensification decomposable process of simulating hydrate；
(4) measured resistivity and CT are imaged：
1. while step (2), (3) are carried out, start resistivity measurement module, determine the resistance in different deposit layers
Value, while being changed by data collecting module collected resistance, temperature, pressure parameter；
2. while above-mentioned parameter is measured, X-CT sweep tests are carried out, obtains the CT figures of system under different experimental conditions
Picture；
3. data reconstruction and analysis are carried out by CT imaging systems, obtains the interior hydration of deposit hole under different experimental conditions
The micro Distribution state of thing, is analyzed with the resistivity containing hydrate sediment for determining, and obtains depositing object
The corresponding relation that the resistivity of system is distributed with hydrate microscopic.
Compared with prior art, advantages and positive effects of the present invention are：
(1) device of the present invention is improved design, the clamper by the structure to ray penetration clamper
Main body uses PEEK materials, and on the one hand the penetrability to X-ray has the compatibility of maximum, on the other hand, it is also possible to greatest extent
Ground mitigates weight of equipment, effectively reduces the burden of X-CT load tables, is conducive to maintaining running accuracy, improves X-CT parsing precision；
Ray penetration clamper can adapt to confined pressure 10MPa, and the working environment of pore pressure (maximum infiltration inlet pressure) 10MPa can
The synthesis of simulating hydrate and decomposable process and measured under the conditions of -5 DEG C-room temperature (covering full sample scope)；
(2) resistivity measurement module launches the receiving pole with electric signal as electric signal successively by four annular electrodes,
6 groups of values of resistivity measurement can be obtained, is measured using relay contacts formula, effectively reduce what interelectrode resistance measurement caused
Error；4 point type resistivity probes are combined by measuring the change in resistance at different sediment core sections, helps to analyze water
The Spatial Variation of resistivity in compound synthesis, decomposable process；
(3) in addition, by temperature control module, the cooperation of constant temperature air bath control cabinet and circulating temperature control system improves temperature control
Precision (± 0.5 DEG C) processed, realizes the experimental analysis that becomes more meticulous, using scanning technique ripe at present, it is ensured that pore communication
The accuracy of test；By the Conjoint Analysis of the microcosmic test results of CT and resistivity macro-test data, to lanthanum chloride hydrate point
The Changing Pattern of resistance parameter has deeper understanding in solution preocess.
Brief description of the drawings
Fig. 1 is ray penetration high pressure clamper and interface diagram described in the embodiment of the present invention 1；
Fig. 2 is the special hydrate measurement apparatus block diagrams of CT described in the embodiment of the present invention 1；
Fig. 3 is combined type multi-point resistivity probe structure schematic diagram described in the embodiment of the present invention 1；
Fig. 4 is the special hydrate measurement apparatus annexation schematic diagrames of CT described in the embodiment of the present invention 1；
1：End cover；2：Cutting ferrule nut；3：Resistivity probe；4：Resistivity probe casing；5：Die sleeve slug；6：Deposition
Thing sample；7：Pressure-bearing pipe；8：Confined pressure fluid intake；9：Pore pressure fluid intake；10：Resistivity probe sleeve and pore pressure fluid issuing
Between annular space；11：Confined pressure fluid issuing；12：Pore pressure fluid issuing；13：Cutting ferrule fixed lobe；14：O-ring seal is installed recessed
Groove；15：Annular electrode；16：Seal convexity；17：Deposit sample glue bucket；18：Ray penetration clamper；19：Pore pressure is vented
Valve；20：Back pressure control valve；21：The plunger displacement pump confined pressure circulatory system；22：Circulating temperature control system；23：Plunger pump priming system；24：
Steel cylinder gas injection system；25：Pressure reduction control valve；26：CT turntables；27：Temperature controller；28：Confined pressure control module；29：Pore pressure control
Molding block；30：Temperature control module；31：Resistivity measurement module；32：CT imaging systems；33：Data acquisition module.
Specific embodiment
In order to be more clearly understood from the above objects, features and advantages of the present invention, below in conjunction with the accompanying drawings and implement
The present invention will be further described for example.
Embodiment 1, with reference to Fig. 2, a kind of special hydrate resistivity test devices of CT, including ray penetration clamper
18th, resistivity measurement module 31, confined pressure control module 28, temperature control module 30, pore pressure control module 29, data acquisition module 33 with
And it is arranged on the CT imaging systems 32 of the both sides of ray penetration clamper 18；The temperature control module 30, confined pressure control module 28 with
And pore pressure control module 29 is connected with ray penetration clamper 18；The data acquisition module 33 respectively with resistivity measurement
Module 31 is connected with CT imaging systems 32.
Described ray penetration clamper 18, specifically refers to coordinate with the transmission imaging turntable of CT imaging systems 32
High pressure resistant clamper, the clamper is the critical component of package unit, specifically, as shown in figure 1, be ray penetration clamping
The structure and interface diagram of device 18：
Ray penetration clamper 18 includes pressure-bearing pipe 7, end cover 1, cutting ferrule nut 2, and pressure-bearing pipe 7 uses PEEK materials
Matter, wall thickness is less than 2mm, and the inside of pressure-bearing pipe 7 is provided with deposit sample glue bucket 17, and the two ends of deposit sample glue bucket 17 are provided with mould
Set slug 5；The two ends lateral wall of pressure-bearing pipe 7 is provided with cutting ferrule fixed lobe 13, the cutting ferrule fixed lobe 13 and cutting ferrule nut 2
Coordinate, end cover 1 is fixed with pressure-bearing pipe 7；The end cover 1 includes being separately positioned on the upper of the two ends of pressure-bearing pipe 7
End cap and bottom end cover, are provided with pore pressure fluid issuing (i.e. pore pressure outflow pipeline) 12 and confined pressure fluid issuing on the upper end cover
11, the pore pressure fluid intake 9 that is connected with pore pressure control module 29 and confined pressure control module 28 is respectively arranged with bottom end cover and is enclosed
Pressure fluid intake 8, and the pore pressure outflow pipeline 12 connected with deposit sample glue bucket is provided with pore pressure outflow pipeline 12.
The resistivity measurement module 31 includes combined type multi-point resistivity probe and resistivity monitoring switching device,
To obtain the resistivity data of sample under different condition；The combined type multi-point resistivity probe includes resistivity probe 3, electricity
Resistance rate probe casing 4 and annular electrode 15, the annular electrode are set in qually spaced on resistivity probe, the resistivity probe
Pipeline is flowed out by pore pressure to be inserted into inside deposit sample, combined type multi-point resistivity probe is placed in ray in practical operation
In deposit inside penetration clamper 18, it is inserted in parallel into clamper wall；The resistivity monitoring switching device, specifically
Refer to the TT＆C software for the detection of combined type multi-point resistivity, the main resistivity sequence measuring that resistance measurement point is provided,
The functions such as automatic storage and retrieval, the setting of electric field stabilization time, the setting of signal source module of database, are the existing of comparative maturity
Technology, is not detailed herein.
(1) 18 main wall pressure-bearing pipe of ray penetration clamper 7 selects PEEK materials, and wall thickness is less than 2mm, pressure-bearing pipe 7
Total length can be adjusted according to the physical length of the physical length of sample and resistivity probe 3, >=70mm, internal diameter 35mm, pressure-bearing
Pipe 7 sets sealing O-ring seal and installs groove 14 near two end faces inwall, is installed inside groove 14 by O-ring seal
Sealing ring realizes the sealing between end cover 1 and pressure-bearing pipe 7；
(2) cutting ferrule nut 2 is the quick cutting ferrule of annular, and material uses stainless steel, and the half the circumference of the sleeve where it joins the shoulder of cutting ferrule nut 2 height is solid with cutting ferrule
Fixed raised 13 match, and the upper-end inner diameter of cutting ferrule nut 2 is equal with the external diameter of end cover 1, can quick locking end cover 1 with hold
Pressure pipe 7；
(3) end cover uses titanium alloy material, and the lower outer diameter of upper end cover is equal with the internal diameter of pressure-bearing pipe 7, bottom end cover
Top external diameter is equal with the internal diameter of pressure-bearing pipe 7, and the sealing function of the sealing ring inside groove 14 is installed with reference to O-ring seal, realizes
Confined pressure chamber is fully sealed with the external world；
(4) interfered between pipeline 12 and confined pressure fluid issuing 11 to prevent pore pressure from flowing out, confined pressure fluid issuing
(i.e. pore pressure outflow pipeline) 11 is internally provided with the hole flowed to upper end cover outer rim, convenient experiment in upper end cover.Similarly, it is anti-
Only pore pressure fluid intake 9 and confined pressure fluid intake 8 are interfered, and confined pressure fluid intake 8 is set specially inside lower end cover
To bottom end cover outer rim flow hole；
(5) pore pressure fluid intake 9, pore pressure outflow pipeline 12 is in the centre of end cover 2, pore pressure fluid injection conduit
Line and pore pressure fluid effuser line are connected with die sleeve slug 5 respectively, realize the injection and output of pore pressure, pore pressure effuser
The internal diameter on road 12 is 4mm, and resistivity probe 3 flows out pipeline 12 and is inserted into inside deposit sample 6 by pore pressure；
(6) combined type multi-point resistivity probe includes resistivity probe 3 and resistivity probe casing 4, resistivity probe
The external diameter of sleeve pipe 4 is 3mm, and the annular space 10 between resistance probe sleeve pipe 4 and pore pressure outflow pipeline 12 goes out as actual apertures hydraulic fluid flow
Passage, resistivity probe 3 sequentially passes through upper end cover, pore pressure outflow pipeline 12, top die sleeve slug 5 and gos deep into deposit from top to bottom
Sample 6, resistivity probe 3 uses thin cylindrical-shaped structure, is the insulator that diameter 3mm length is 50mm, and it is in deposit sample 6
In actually active length be 40mm, resistivity probe 3 installs resistance in the effective length in deposit sample 6 every 10mm
Rate annular electrode 15, each annular electrode both can be as electron emitter, it is also possible to used as electronic receipt pole, thus can be with
Measurement deposit internal resistance rate value amounts to C4 2=6 groups；And the switching of Resistance probe, using the relay contacts formula knot of resistance stabilization
Structure, because in absolute separation electrically, the resistance stabilization of relay mechanical contact will not be brought to interelectrode resistance measurement
Error；
According to the location of annular electrode 15, the specific resistivity measurement of combined type multi-point resistivity probe is interval such as
Shown in accompanying drawing 3, minimum resistance measurement range 10mm, maximum resistance measurement range 30mm, 6 resistivity values reflect that difference is cutd open respectively
Resistivity average value on face, 6 resistivity spatial arrangements can observe the sky of resistivity in lanthanum chloride hydrate and decomposable process
Between Changing Pattern.
(7) die sleeve slug 5 is stainless steel, designs seal convexity 16 at two on die sleeve slug 5, die sleeve slug 5 with it is heavy
Interference fit connection between product thing sample glue bucket 17, sealing deposit sample 6, the Main Function of the seal convexity 16 is into one
The two ends sealing of step enhanced deposition thing sample 6, prevents pore pressure, confined pressure from ganging up；Hydrate sediment sample 6 is the examination of fabricated in situ
Sample, specimen length >=50mm, specimen finish 25mm；
(8) resistance probe sleeve pipe 4 uses the expanded range of hard insulation, resistance probe sleeve pipe 4 to enter from resistance probe
Enter pore pressure outflow pipeline 12 arrived through top die sleeve slug 5, the resistivity probe 3 of deposit inside extension does not wrap up resistance
Probe casing 4.
With reference to Fig. 4, the confined pressure control module 28 includes the plunger displacement pump confined pressure circulatory system 21 and Back pressure control valve 15, confined pressure
Control module 28 is connected by the confined pressure fluid intake 8 on the end cover 2 of ray penetration clamper 18 with clamper, plunger displacement pump
The confined pressure circulatory system 21 is connected by Back pressure control valve 15 with the end of confined pressure fluid issuing 11, using the plunger displacement pump confined pressure circulatory system 21
Pressure source is provided, coordinates Back pressure control valve 15, realize that system confined pressure is controlled, confined pressure maximum 10MPa；Back pressure control valve 15 is by calculating
Machine is automatically controlled, and can be set the height of confined pressure and be automatically controlled, and confined pressure control accuracy reaches 0.1FS；
The temperature control module 30 includes temperature controller 27 and circulating temperature control system 22, and wherein temperature controller 27 is constant temperature
Air bath control cabinet, all of device is all placed in the constant temperature air bath control cabinet and is tested；Loop temperature-control system 27 and post
The injection pipeline connection of the plug pump confined pressure circulatory system 21, for controlling the temperature in fluid circuit, makes ray penetration clamper
Can be realized temperature control at import between -5 DEG C-room temperature；Under the collective effect of both, realize temperature-controlled precision ±
0.5 DEG C, the Main Function of temperature control module is the temperature conditionss for controlling lanthanum chloride hydrate to decompose.
The sample interior pore pressure control module 32 includes plunger pump priming system 23, steel cylinder gas injection system 24 and decompression
Control valve 25 etc., wherein, steel cylinder gas injection system 24 and Decompression Controlling method 25 are mainly used in injecting gases at high pressure to sample interior；Post
The main liquid system 23 of plug pump is used for sample interior with constant flow rate or constant pressure injection liquid.Plunger pump priming system and steel cylinder
Gas injection system mixes injection before clamper pore pressure entrance, both pressure balances is controlled by pressure reduction control valve 25, it is to avoid gas
Body pours into plunger pump priming system or liquid enters steel cylinder gas injection system.
CT imaging systems described in the present embodiment 32 is VtomexnanotomCT imaging systems, its application method and basic
It is formed in publication number CN202676633U and has been discussed in detail, will not be described here.The present invention is using the system as deposit
The basic means of pore communication parameter testing, the nucleus equipment of data acquisition module 33 is aglient data acquisition units, can be real
The Automatic Control that reality is tested, resistivity data automatic acquisition and processing；And can be with the seamless companies of CT system Vtomexnanotom
Connect；By software and the data-interface of aglient, the time lag of resistance measurement can be set, capacitive reactance pair is suppressed in measurement
The influence of measurement result；Software is write using labview, and the general driving interface of labview is provided due to aglient equipment,
There is great robustness using the program of the software programming.The Main Function of data acquisition module is that Real-time Collection hydrate is closed
Into the resistance parameter in decomposable process, pore communication parameter, hydrate concentration, dissolved gas saturation degree and water saturation
Running parameter, and carry out correlation data processing, obtain resistance parameter and porosity communication in lanthanum chloride hydrate decomposable process
Property couple variations rule.
In the present embodiment, ray penetration clamper is placed on X-CT objective tables, clamper is swept by X-ray
Retouch, obtain the CT images under different condition, obtain the micro Distribution of hydrate in deposit hole；By data acquisition module to body
The various parameters (temperature, pressure, gas flow, resistivity etc.) of system carry out Real-time Collection and analysis.
Embodiment 2, based on the device described in embodiment 1, the present embodiment is disclosed directly below measuring method：
(1) dress sample and installation：
1. ray penetration clamper is opened, deposit is filled up in deposit sample glue bucket and is added the appropriate aqueous solution；
2. resistivity probe casing and resistivity probe, end cover are inserted；
3. ray penetration clamper is installed on CT imaging system objective tables；
(2) gas hydrates are generated：
1. temperature control module switch is opened, circulating water temperature is set, make sediment sample temperature in ray penetration clamper
Reach the temperature requirements of experiment；
2. setting liquid is injected to sample interior to setting pressure by piston pump liquid injection system；Regulation pressure reduction control valve,
Add reacting gas so that the pressure needed for pressure reaches experiment in ray penetration clamper；
3. pressure source is provided using the plunger displacement pump confined pressure circulatory system, coordinates Back pressure control valve, needed for realizing system experimentation
System confined pressure；Because there is provided suitable temperature, pressure condition, gas hydrates start generation, and are progressively filled into deposition
In thing hole；
(3) gas hydrate dissociation is simulated：
1. after step (2) is fully finished, temperature control module continuous firing is kept；Pore pressure inlet valve is closed, is progressively opened
The valve of pore pressure fluid issuing, simulating hydrate step-down decomposable process；Or
2. pore pressure fluid inlet valve is closed, is gradually heated up to system by temperature control module, and by controlling pore pressure fluid
Outlet valve realizes that the pressure inside ray penetration clamper is in steady state, the intensification decomposable process of simulating hydrate；
(4) measured resistivity and CT are imaged：
1. while step (2), (3) are carried out, start resistivity measurement module, determine the resistance in different deposit layers
Value, while being changed by data collecting module collected resistance, temperature, pressure parameter；
2. while above-mentioned parameter is measured, X-CT sweep tests are carried out, obtains the CT figures of system under different experimental conditions
Picture；
3. data reconstruction and analysis are carried out by CT imaging systems, obtains the interior hydration of deposit hole under different experimental conditions
The micro Distribution state of thing, is analyzed with the resistivity containing hydrate sediment for determining, and obtains depositing object
The corresponding relation that the resistivity of system is distributed with hydrate microscopic.
The above, is only presently preferred embodiments of the present invention, is not the limitation for making other forms to the present invention, is appointed
What those skilled in the art changed possibly also with the technology contents of the disclosure above or be modified as equivalent variations etc.
Effect embodiment is applied to other fields, but every without departing from technical solution of the present invention content, according to technical spirit of the invention
Any simple modification, equivalent variations and the remodeling made to above example, still fall within the protection domain of technical solution of the present invention.
Claims (10)
- The special hydrate resistivity test devices of 1.CT, it is characterised in that including ray penetration clamper, resistivity measurement mould Block, confined pressure control module, temperature control module, pore pressure control module, data acquisition module and it is arranged on ray penetration clamper The CT imaging systems of both sides；The temperature control module, confined pressure control module and pore pressure control module are clamped with ray penetration Device is connected；The data acquisition module is connected with resistivity measurement module and CT imaging systems respectively；The ray penetration clamper includes pressure-bearing pipe, end cover, cutting ferrule nut, and pressure-bearing pipe uses PEEK materials, wall thickness Less than 2mm, the inside of pressure-bearing pipe is provided with deposit sample glue bucket, and the two ends of deposit sample glue bucket are provided with die sleeve slug；Pressure-bearing The two ends lateral wall of pipe is provided with cutting ferrule fixed lobe, the cutting ferrule fixed lobe and cutting ferrule nut screw connection, by end cover with Pressure-bearing pipe is fixed；The end cover includes being separately positioned on the upper end cover and bottom end cover at pressure-bearing pipe two ends, the upper end Cover and be provided with pore pressure fluid issuing and confined pressure fluid issuing, be respectively arranged with bottom end cover and pore pressure control module and confined pressure control Molding block connected pore pressure fluid intake and confined pressure fluid intake, and be provided with pore pressure fluid issuing and deposit sample glue bucket The pore pressure outflow pipeline of connection；The resistivity measurement module includes combined type multi-point resistivity probe and resistivity monitoring switching device, to obtain The resistivity spatial distribution data of sample under different condition；The combined type multi-point resistivity probe include resistivity probe, Resistivity probe casing and annular electrode, the annular electrode are set in qually spaced on resistivity probe, the resistivity probe Pipeline is flowed out by pore pressure to be inserted into inside deposit sample.
- 2. measurement apparatus according to claim 1, it is characterised in that：The confined pressure control module is followed including plunger displacement pump confined pressure Loop systems and Back pressure control valve, the plunger displacement pump confined pressure circulatory system are connected by Back pressure control valve with confined pressure fluid outlet.
- 3. measurement apparatus according to claim 1, it is characterised in that：The temperature control module includes constant temperature air bath control cabinet And circulating temperature control system, loop temperature-control system is connected with the injection pipeline of the plunger displacement pump confined pressure circulatory system.
- 4. measurement apparatus according to claim 1, it is characterised in that：The pore pressure control module includes plunger displacement pump fluid injection system System, steel cylinder gas injection system and pressure reduction control valve, the steel cylinder gas injection system pass through pressure reduction control valve and plunger pump priming system phase Even, then it is commonly connected to pore pressure fluid inlet end.
- 5. measurement apparatus according to claim 1, it is characterised in that：The resistivity probe is being inserted into deposit sample In actually active length be 40mm, the annular electrode include 4, the distance between adjacent annular electrode be 10mm.
- 6. measurement apparatus according to claim 5, it is characterised in that：The external diameter of the resistivity probe casing is 3mm, is adopted With hard insulation, the annular space between resistance probe sleeve pipe and pore pressure outflow pipeline goes out passage for actual apertures hydraulic fluid flow.
- 7. measurement apparatus according to claim 1, it is characterised in that：It is provided with the die sleeve slug at two and seals convex Rise, interference fit between die sleeve slug and deposit sample glue bucket.
- 8. measurement apparatus according to claim 1, it is characterised in that：Set between the pressure-bearing pipe madial wall and end cover It is equipped with O-ring seal mounting groove.
- 9. measurement apparatus according to claim 1, it is characterised in that：Described pore pressure fluid intake, pore pressure fluid issuing The center of end cover is arranged at, and respectively by pore pressure fluid inlet line and pore pressure fluid issuing pipeline and die sleeve section Plug is connected.
- 10. the measuring method of measurement apparatus described in a kind of utilization claim 1, it is characterised in that comprise the following steps：(1) dress sample and installation：1. ray penetration clamper is opened, deposit is filled up in deposit sample glue bucket and is added the appropriate aqueous solution；2. resistivity probe casing and resistivity probe, end cover are inserted；3. ray penetration clamper is installed on CT imaging system objective tables；(2) gas hydrates are generated：1. temperature control module switch is opened, circulating water temperature is set, reach sediment sample temperature in ray penetration clamper The temperature requirements of experiment；2. setting liquid is injected to sample interior to setting pressure by piston pump liquid injection system；Regulation pressure reduction control valve, adds Reacting gas so that the pressure needed for pressure reaches experiment in ray penetration clamper；3. pressure source is provided using the plunger displacement pump confined pressure circulatory system, coordinates Back pressure control valve, the system needed for realizing system experimentation Confined pressure；Because there is provided suitable temperature, pressure condition, gas hydrates start generation, and are progressively filled into deposit hole In gap；(3) gas hydrate dissociation is simulated：1. after step (2) is fully finished, temperature control module continuous firing is kept；Pore pressure inlet valve is closed, pore pressure is progressively opened The valve of fluid issuing, simulating hydrate step-down decomposable process；Or2. pore pressure fluid inlet valve is closed, is gradually heated up to system by temperature control module, and by controlling pore pressure fluid issuing Valve realizes that the pressure inside ray penetration clamper is in steady state, the intensification decomposable process of simulating hydrate；(4) measured resistivity and CT are imaged：1. while step (2), (3) are carried out, start resistivity measurement module, determine the resistance value in different deposit layers, Changed by data collecting module collected resistance, temperature, pressure parameter simultaneously；2. while above-mentioned parameter is measured, X-CT sweep tests are carried out, obtains the CT images of system under different experimental conditions；3. data reconstruction and analysis are carried out by CT imaging systems, hydrate in deposit hole under acquisition different experimental conditions Micro Distribution state, is analyzed with the resistivity containing hydrate sediment for determining, and obtains sediment The corresponding relation that resistivity is distributed with hydrate microscopic.
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