CN106872497B - 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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- CN106872497B CN106872497B CN201710303350.9A CN201710303350A CN106872497B CN 106872497 B CN106872497 B CN 106872497B CN 201710303350 A CN201710303350 A CN 201710303350A CN 106872497 B CN106872497 B CN 106872497B
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000012360 testing method Methods 0.000 title claims abstract description 17
- 239000000523 sample Substances 0.000 claims abstract description 105
- 239000011148 porous material Substances 0.000 claims abstract description 89
- 239000012530 fluid Substances 0.000 claims abstract description 67
- 230000035515 penetration Effects 0.000 claims abstract description 44
- 238000005259 measurement Methods 0.000 claims abstract description 29
- 238000013170 computed tomography imaging Methods 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 17
- 239000013049 sediment Substances 0.000 claims abstract description 17
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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
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- 229910000831 Steel Inorganic materials 0.000 claims description 11
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- 150000004677 hydrates Chemical class 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
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- 238000009434 installation Methods 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 5
- 230000006837 decompression Effects 0.000 claims description 5
- 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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- 238000010304 firing Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
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- 230000008859 change Effects 0.000 description 11
- 230000008021 deposition Effects 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 outlet and confined pressure fluid outlet are provided with upper end cover, pore pressure fluid inlet and confined pressure fluid inlet are provided with bottom end cover；Resistivity measurement module includes resistivity probe, resistivity probe casing and annular electrode etc., and annular electrode is set in qually spaced on resistivity probe.By the device not only can Accurate Determining hydrate generate decomposable process in resistivity Spatial Variation, but also can realize X CT scan be imaged, so as to fulfill 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, the ocean shelf margin being mainly distributed on below 300 meters of the depth of water
A kind of or dirt band area, it is considered to be 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
Obvious change occurs for compound, its resistance characteristic, and therefore, electrology characteristic is the main physical parameter of hydrate reservoir.Pass through survey
Measure the change in resistance in bottom sediment stratum, you can judge hydrate reservoir, further satisfy 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, utilizes difference
Electrode or sensor, sediment in high-voltage penetration clamper or different layers position are tested, the result is that
Whole system or the average resistance change of some layer of position, since 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 cannot accurately portray hydrate storage shape
State and its influence of the distribution situation to resistivity in deposit hole；It can not reflect hydrate micro Distribution inside deposit
Influence of the condition to resistivity, can not especially judge change in resistance rule and deposition in lanthanum chloride hydrate or generating process
The response pattern of thing pore throat Parameters variation, can not explain change in resistance in hydrate generation, decomposable process from micro-scale
Mechanism.
In fact, during gas hydrates generate or decompose, the dissolving in deposit pore communication, hole
Gas, water and ion concentration can all change, and these are exactly the principal element for changing reaction medium electric conductivity.It is being hydrated
In terms of the detection of sediment microstructure, also there is relevant research in the country：As publication number CN102636503B discloses a kind of day
The right natural core CT of gas hydrate reforms special ray penetration clamper and method；Publication number CN101246117B and
It is micro- with CT that the patent of invention of CN104155188B will contain hydrate sediment mechanics parameter measuring device 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 it there is no shout what structure detection was combined with the microcosmic hole containing hydrate sediment specifically 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
The dependency relation hindered between 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, and the experiment of the situation of change of deposit pore communication, hydrate, dissolved gas and water can be observed at the same time
Test device and method, are estimated with hydrate concentration dependency relation, raising hydrate stock number obtaining reliable resistivity
Accuracy it is significant, it helps explain that resistance parameter change is advised in lanthanum chloride hydrate and decomposable process from 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 really resistivity in measure hydrate generation decomposable process, and X-CT scanning imageries can be realized at the same time, so as to observe deposit hole
Gap connectedness, hydrate, the situation of change of dissolved gas and water, realize hydrate sediment system resistivity and porosity communication
The synchro measure of property.
The present invention is realized using following technical solution：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 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 pressure-bearing pipe is internally provided with deposit sample glue bucket, and the both ends of deposit sample glue bucket are equipped with die sleeve slug；
The both ends lateral wall of pressure-bearing pipe is equipped with cutting ferrule fixed lobe, and the cutting ferrule fixed lobe coordinates with cutting ferrule nut, by sealed end
Lid is fixed with pressure-bearing pipe；The end cover includes the upper end cover and bottom end cover for being separately positioned on pressure-bearing pipe both ends, described
Pore pressure fluid outlet and confined pressure fluid outlet are provided with upper end cover, is respectively arranged with and pore pressure control module and encloses on bottom end cover
The pore pressure fluid inlet and confined pressure fluid inlet that pressure control module is connected, and be equipped with and deposit sample in pore pressure fluid outlet
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
Obtain the resistivity data of sample under 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 pump confined pressure circulatory system and Back pressure control valve, and plunger 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 pump confined pressure circulatory system
Source, coordinates Back pressure control valve to realize that system confined pressure controls, 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
It is connected with the injection pipeline of the plunger pump confined pressure circulatory system, for controlling the temperature in fluid circuit, clamps ray penetration
Device entrance can be realized 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 inlet
End, plunger pump priming system and steel cylinder gas injection system mixed injection before ray penetration clamper pore pressure fluid inlet, and lead to
Pressure reduction control valve control both pressure balance is crossed, avoids that 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 can both be used as electron emission
Pole, can also be used 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 outside diameter of the resistivity probe casing is 3mm, using hard insulation, resistance probe casing
The annular space flowed out with pore pressure between pipeline goes out passage for actual apertures hydraulic fluid flow.
Further, be provided with seal convexity at two on the die sleeve slug, die sleeve slug and deposit sample glue bucket it
Between be interference fitted, seal deposit sample, to further enhance deposit sample both ends leakproofness, 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
Sealing ring inside circle installation groove realizes the sealing between end cover and pressure-bearing pipe.
Further, the pore pressure fluid inlet, pore pressure fluid outlet are arranged at the center of end cover, and divide
Be not connected by pore pressure fluid inlet line and pore pressure fluid outlet pipeline with die sleeve slug, realize pore pressure injection and
Output.
Further, to prevent the fixing nut between pore pressure fluid outlet and confined pressure fluid outlet from interfering,
And preventing pore pressure fluid inlet and confined pressure fluid inlet from interfering, the confined pressure fluid outlet is internally provided with upper end cover
The hole flowed to end cover outer rim, and confined pressure fluid inlet is internally provided with the hole flowed to bottom end cover outer rim in bottom end cover
Gap, convenient experiment.
In addition a kind of measuring method using the special hydrate resistivity test devices of above-mentioned CT is also disclosed in the present invention, including
Following steps：
(1) sample and installation are filled：
1. opening ray penetration clamper, fill up deposit in deposit sample glue bucket and add appropriate aqueous solution；
2. it is inserted into resistivity probe casing and resistivity probe, end cover；
3. ray penetration clamper is installed on CT imaging system objective tables；
(2) gas hydrates are generated：
1. opening temperature control module switch, circulating water temperature is set, makes 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；Adjust pressure reduction control valve,
Add reacting gas so that pressure reaches the pressure needed for experiment in ray penetration clamper；
3. providing pressure source using the plunger pump confined pressure circulatory system, coordinate Back pressure control valve, realize needed for system experimentation
System confined pressure；Due to providing suitable temperature, pressure condition, gas hydrates start to generate, 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 outlet, simulating hydrate decompression decomposable process；Or
2. closing pore pressure fluid inlet valve, gradually heated up by temperature control module to system, and by controlling pore pressure fluid
Outlet valve realizes that the pressure inside ray penetration clamper is in steady state, the heating decomposable process of simulating hydrate；
(4) measured resistivity and CT imagings：
1. carried out in step (2), (3), start resistivity measurement module, measure the resistance in different deposit layers
Value, while changed by data collecting module collected resistance, temperature, pressure parameter；
2. while above-mentioned parameter measures, X-CT sweep tests are carried out, obtain the CT figures of system under different experimental conditions
Picture；
3. carrying out data reconstruction and analysis by CT imaging systems, hydration in deposit hole under different experimental conditions is obtained
The micro Distribution state of thing, compares and analyzes with the resistivity of the sediment containing hydrate of measure, obtains deposition object
The resistivity of system and the correspondence of hydrate microscopic distribution.
Compared with prior art, the advantages and positive effects of the present invention are：
(1) device of the present invention to the structure of ray penetration clamper by being improved design, the clamper
Main body uses PEEK materials, on the one hand has the compatibility of maximum to the penetrability of X-ray, on the other hand, can also be to greatest extent
Ground mitigates weight of equipment, effectively reduces the burden of X-CT load tables, is conducive to maintain 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 is used as the receiving pole of electric signal transmitting and electric signal by four annular electrodes successively,
The value of 6 groups of resistivity measurements can be obtained, is measured, is effectively reduced caused by interelectrode resistance measurement using relay contacts formula
Error；4 point type resistivity probes are combined by measuring the change in resistance at different sediment core sections, help 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, and using scanning technique ripe at present, ensures 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 rule 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 measuring device 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 measuring device connection relationship diagrams 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 inlet；9：Pore pressure fluid inlet；10：Resistivity probe sleeve and pore pressure fluid outlet
Between annular space；11：Confined pressure fluid outlet；12：Pore pressure fluid outlet；13：Cutting ferrule fixed lobe；14：O-ring seal installation is 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 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.
Embodiment
In order to which the above objects, features and advantages of the present invention is more clearly understood, below in conjunction with the accompanying drawings and implement
The present invention will be further described for example.
Embodiment 1, with reference to figure 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 18 both sides of ray penetration clamper；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.
The ray penetration clamper 18, in particular to it can coordinate with the transmission imaging turntable of CT imaging systems 32
High pressure resistant clamper, which is the critical component of package unit, specifically, as shown in Figure 1, for ray penetration clamp
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 are less than 2mm, and pressure-bearing pipe 7 is internally provided with deposit sample glue bucket 17, and the both ends of deposit sample glue bucket 17 are equipped with mould
Cover slug 5；The both ends lateral wall of pressure-bearing pipe 7 is equipped with cutting ferrule fixed lobe 13, the cutting ferrule fixed lobe 13 and cutting ferrule nut 2
Coordinate, end cover 1 and pressure-bearing pipe 7 are fixed；The end cover 1 includes being separately positioned on the upper of 7 both ends of pressure-bearing pipe
End cap and bottom end cover, pore pressure fluid outlet (i.e. pore pressure outflow pipeline) 12 and confined pressure fluid outlet are provided with the upper end cover
11, the pore pressure fluid inlet 9 being connected with pore pressure control module 29 and confined pressure control module 28 is respectively arranged with bottom end cover and is enclosed
Fluid inlet 8 is pressed, and the pore pressure connected with deposit sample glue bucket is equipped with pore pressure outflow pipeline 12 and flows out 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 the automatic storage and retrieval of database, electric field stabilization time are set, the setting of signal source module, are the existing of comparative maturity
Technology, it is not described here in detail.
(1) 18 main wall pressure-bearing pipe 7 of ray penetration clamper 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 sample and the physical length of resistivity probe 3, >=70mm, internal diameter 35mm, pressure-bearing
Pipe 7 sets sealing O-ring seal installation groove 14 close to two end faces inner wall, inside O-ring seal installation groove 14
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 circular ring shape, and material uses stainless steel, and 2 half the circumference of the sleeve where it joins the shoulder of cutting ferrule nut height is consolidated with cutting ferrule
Fixed protrusion 13 matches, and 2 upper-end inner diameter of cutting ferrule nut is equal with 1 outside diameter of end cover, 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 7 internal diameter of pressure-bearing pipe, bottom end cover
Top outside diameter is equal with 7 internal diameter of pressure-bearing pipe, with reference to the sealing function of the sealing ring inside O-ring seal installation groove 14, realizes
Confined pressure chamber is fully sealed with extraneous；
(4) interfered to prevent pore pressure from flowing out between pipeline 12 and confined pressure fluid outlet 11, confined pressure fluid outlet
(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 inlet 9 and confined pressure fluid inlet 8 interfere, and confined pressure fluid inlet 8 is set specially inside lower end cover
To bottom end cover outer rim flow hole；
(5) pore pressure fluid inlet 9, pore pressure outflow pipeline 12 are in the centre of end cover 2, pore pressure fluid injection conduit
Line and pore pressure fluid outflow pipeline 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 by pore pressure and is inserted into inside deposit sample 6；
(6) combined type multi-point resistivity probe includes resistivity probe 3 and resistivity probe casing 4, resistivity probe
The outside diameter of casing 4 is 3mm, and the annular space 10 between resistance probe casing 4 and pore pressure outflow pipeline 12 goes out as actual apertures hydraulic fluid flow
Passage, resistivity probe 3 sequentially pass through upper end cover, pore pressure outflow pipeline 12, top die sleeve slug 5 and go deep into deposit from top to bottom
Sample 6, resistivity probe 3 use thin cylindrical-shaped structure, are the insulator that diameter 3mm length is 50mm, 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 can both be used as electron emitter, can also be 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, due to stablizing, will not be brought to interelectrode resistance measurement in absolute separation electrically, the resistance value of relay mechanical contact
Error；
According to the location of annular electrode 15, the specific resistivity measurement section of combined type multi-point resistivity probe is such as
Shown in attached 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 rule.
(7) die sleeve slug 5 is stainless steel, seal convexity 16 at two is designed on die sleeve slug 5, die sleeve slug 5 is with sinking
Connection is interference fitted between product thing sample glue bucket 17, sealing deposit sample 6, the main function of the seal convexity 16 is into one
6 both ends leakproofness of enhanced deposition thing sample is walked, 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 casing 4 uses hard insulation, the expanded range of resistance probe casing 4 from resistance probe into
Enter pore pressure and flow out pipeline 12 untill through top die sleeve slug 5, deposit extends internally resistivity probe 3 and do not wrap up resistance
Probe casing 4.
With reference to figure 4, the confined pressure control module 28 includes the plunger pump confined pressure circulatory system 21 and Back pressure control valve 15, confined pressure
Control module 28 is connected by the confined pressure fluid inlet 8 on 18 end cover 2 of ray penetration clamper with clamper, plunger pump
The confined pressure circulatory system 21 is connected by Back pressure control valve 15 with 11 end of confined pressure fluid outlet, utilizes the plunger pump confined pressure circulatory system 21
Pressure source is provided, coordinates Back pressure control valve 15, realizes that system confined pressure controls, confined pressure maximum 10MPa；Back pressure control valve 15 is by calculating
Machine automatically controls, and can set the height of confined pressure and automatically control, 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 devices are all placed in the constant temperature air bath control cabinet and are tested；Loop temperature-control system 27 and column
The injection pipeline connection of the plug pump confined pressure circulatory system 21, for controlling the temperature in fluid circuit, makes ray penetration clamper
Entrance can be realized temperature control 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 for injecting gases at high pressure to sample interior；Column
Plug pumps main liquid system 23 and is used to inject liquid to sample interior with constant flow rate or constant pressure.Plunger pump priming system and steel cylinder
Gas injection system mixed injection before clamper pore pressure entrance, by both pressure balances of the control of pressure reduction control valve 25, avoids 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, this will not be repeated here.The present invention is used as deposit using the system
The basic means of pore communication parameter testing, the core equipment of data acquisition module 33 is aglient data collectors, 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, suppress capacitive reactance pair in measurement
The influence of measurement result；Software is write using labview, since aglient equipment provides the general driving interface of labview,
There is great robustness using the program of the software programming.The main function of data acquisition module is that real-time collection hydrate closes
Into the resistance parameter in decomposable process, pore communication parameter, hydrate concentration, dissolved gas saturation degree and water saturation
Running parameter, and carry out relevant 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 gather and analyze in real time.
Embodiment 2, based on the device described in embodiment 1, the present embodiment is disclosed directly below measuring method：
(1) sample and installation are filled：
1. opening ray penetration clamper, fill up deposit in deposit sample glue bucket and add appropriate aqueous solution；
2. it is inserted into resistivity probe casing and resistivity probe, end cover；
3. ray penetration clamper is installed on CT imaging system objective tables；
(2) gas hydrates are generated：
1. opening temperature control module switch, circulating water temperature is set, makes 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；Adjust pressure reduction control valve,
Add reacting gas so that pressure reaches the pressure needed for experiment in ray penetration clamper；
3. providing pressure source using the plunger pump confined pressure circulatory system, coordinate Back pressure control valve, realize needed for system experimentation
System confined pressure；Due to providing suitable temperature, pressure condition, gas hydrates start to generate, 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 outlet, simulating hydrate decompression decomposable process；Or
2. closing pore pressure fluid inlet valve, gradually heated up by temperature control module to system, and by controlling pore pressure fluid
Outlet valve realizes that the pressure inside ray penetration clamper is in steady state, the heating decomposable process of simulating hydrate；
(4) measured resistivity and CT imagings：
1. carried out in step (2), (3), start resistivity measurement module, measure the resistance in different deposit layers
Value, while changed by data collecting module collected resistance, temperature, pressure parameter；
2. while above-mentioned parameter measures, X-CT sweep tests are carried out, obtain the CT figures of system under different experimental conditions
Picture；
3. carrying out data reconstruction and analysis by CT imaging systems, hydration in deposit hole under different experimental conditions is obtained
The micro Distribution state of thing, compares and analyzes with the resistivity of the sediment containing hydrate of measure, obtains deposition object
The resistivity of system and the correspondence of hydrate microscopic distribution.
The above described is only a preferred embodiment of the present invention, being not the limitation for making other forms to the present invention, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Effect embodiment is applied to other fields, but every without departing from technical solution of the present invention content, the technical spirit according to the present 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, pressure-bearing pipe is internally provided with deposit sample glue bucket, and the both ends of deposit sample glue bucket are equipped with die sleeve slug；Pressure-bearing The both ends lateral wall of pipe is equipped with cutting ferrule fixed lobe, and the cutting ferrule fixed lobe coordinates with cutting ferrule nut, by end cover with Pressure-bearing pipe is fixed；The end cover includes the upper end cover and bottom end cover for being separately positioned on pressure-bearing pipe both ends, the upper end Cover and be provided with pore pressure fluid outlet and confined pressure fluid outlet, be respectively arranged with bottom end cover and pore pressure control module and confined pressure control The pore pressure fluid inlet and confined pressure fluid inlet that molding block is connected, and be equipped with and deposit sample glue bucket in pore pressure fluid outlet 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. measuring device according to claim 1, it is characterised in that：The confined pressure control module is followed including plunger pump confined pressure Loop system and Back pressure control valve, the plunger pump confined pressure circulatory system are connected by Back pressure control valve with confined pressure fluid outlet.
- 3. measuring device 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 are connected with the injection pipeline of the plunger pump confined pressure circulatory system.
- 4. measuring device according to claim 1, it is characterised in that：The pore pressure control module includes plunger 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. measuring device 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 includes 4, and the distance between adjacent annular electrode is 10mm.
- 6. measuring device according to claim 5, it is characterised in that：The outside diameter of the resistivity probe casing is 3mm, is adopted With hard insulation, the annular space between resistance probe casing and pore pressure outflow pipeline goes out passage for actual apertures hydraulic fluid flow.
- 7. measuring device according to claim 1, it is characterised in that：It is convex that sealing at two is provided with the die sleeve slug Rise, be interference fitted between die sleeve slug and deposit sample glue bucket.
- 8. measuring device 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. measuring device according to claim 1, it is characterised in that：The pore pressure fluid inlet, pore pressure fluid outlet The center of end cover is arranged at, and passes through pore pressure fluid inlet line and pore pressure fluid outlet pipeline and die sleeve section respectively Plug is connected.
- 10. a kind of measuring method using measuring device described in claim 1, it is characterised in that comprise the following steps：(1) sample and installation are filled：1. opening ray penetration clamper, fill up deposit in deposit sample glue bucket and add appropriate aqueous solution；2. it is inserted into resistivity probe casing and resistivity probe, end cover；3. ray penetration clamper is installed on CT imaging system objective tables；(2) gas hydrates are generated：1. opening temperature control module switch, circulating water temperature is set, reaches 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；Pressure reduction control valve is adjusted, is added Reacting gas so that pressure reaches the pressure needed for experiment in ray penetration clamper；3. providing pressure source using the plunger pump confined pressure circulatory system, coordinate Back pressure control valve, realize the system needed for system experimentation Confined pressure；Due to providing suitable temperature, pressure condition, gas hydrates start to generate, 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, progressively opens pore pressure The valve of fluid outlet, simulating hydrate decompression decomposable process；Or2. closing pore pressure fluid inlet valve, gradually heated up by temperature control module to system, and by controlling pore pressure fluid outlet Valve realizes that the pressure inside ray penetration clamper is in steady state, the heating decomposable process of simulating hydrate；(4) measured resistivity and CT imagings：1. carried out in step (2), (3), start resistivity measurement module, measure the resistance value in different deposit layers, Changed at the same time by data collecting module collected resistance, temperature, pressure parameter；2. while above-mentioned parameter measures, X-CT sweep tests are carried out, obtain the CT images of system under different experimental conditions；3. carrying out data reconstruction and analysis by CT imaging systems, hydrate in deposit hole is obtained under different experimental conditions Micro Distribution state, compares and analyzes with the resistivity of the sediment containing hydrate of measure, obtains sediment Resistivity and the correspondence of hydrate microscopic distribution.
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| CN109655373B (en) * | 2018-12-25 | 2024-05-10 | 国家地质实验测试中心 | Natural gas hydrate reservoir in-situ property parameter simulation test method |
| CN110487607B (en) * | 2019-08-20 | 2020-08-04 | 青岛海洋地质研究所 | Multi-type hydrate generation monitoring and testing method |
| CN114459910A (en) * | 2020-10-22 | 2022-05-10 | 中国石油化工股份有限公司 | Hydrate core testing method and device |
| CN114965579A (en) * | 2021-02-24 | 2022-08-30 | 中国石油化工股份有限公司 | Oil, gas and water three-phase fluid saturation calibration test device and method |
| CN113049465B (en) * | 2021-03-09 | 2022-08-26 | 中国地质科学院水文地质环境地质研究所 | Device and method for simulating water texture characteristics under frozen soil degradation condition |
| CN114526983B (en) * | 2022-02-18 | 2023-02-10 | 西湖大学 | Confining pressure and temperature control integrated system for multi-field coupling in-situ experiment instrument |
| CN114526984B (en) * | 2022-02-18 | 2024-04-05 | 西湖大学 | Multi-field coupling in-situ experiment instrument |
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| CN101246117B (en) * | 2008-03-25 | 2011-04-20 | 中国科学院力学研究所 | Gas-hydrate synthesizing and macro-microscopic mechanics nature synthetic experiment system |
| CN102636503B (en) * | 2011-11-24 | 2014-04-02 | 大连理工大学 | CT (Electronic Computed X-ray Tomography technique) reformer for natural gas hydrate nature core and using method thereof |
| CN102519991B (en) * | 2011-12-20 | 2013-11-06 | 大连理工大学 | Natural gas hydrate heat transfer performance testing apparatus used in X-ray CT equipment |
| CN203365579U (en) * | 2013-07-08 | 2013-12-25 | 青岛海洋地质研究所 | Apparatus for measuring electrical parameters of natural gas hydrate in deposit |
| CN105424734B (en) * | 2016-01-12 | 2018-04-10 | 大连理工大学 | A kind of cryogenic high pressure control device generated for X ray CT equipment observation water compound with resolution characteristic |
| CN205426212U (en) * | 2016-02-03 | 2016-08-03 | 青岛海洋地质研究所 | Many physics of gas hydrate exploitation field evolution simulating measurement setup |
| CN106290421B (en) * | 2016-09-14 | 2018-12-21 | 大连理工大学 | A kind of hydrate growth rate and effective volume measuring device and method based on Microfocus X-ray X ray CT |
| CN206772864U (en) * | 2017-05-03 | 2017-12-19 | 青岛海洋地质研究所 | The special hydrate resistivity test devices of CT |
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