CN104407233B - Hydrate dielectric property test device in a kind of deposit - Google Patents
Hydrate dielectric property test device in a kind of deposit Download PDFInfo
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- CN104407233B CN104407233B CN201410722729.XA CN201410722729A CN104407233B CN 104407233 B CN104407233 B CN 104407233B CN 201410722729 A CN201410722729 A CN 201410722729A CN 104407233 B CN104407233 B CN 104407233B
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Abstract
The present invention discloses hydrate dielectric property test device in a kind of deposit, including built-in reactor, air supply system, pumped vacuum systems, data collecting system, temperature control system and TT＆C system, the TT＆C system includes Q tables and anti-interference shielding line, also include retrievable capacity measurement room, first cylindrical electrode, second cylindrical electrode and tin film, sample carrier sheet is provided with the middle of retrievable electric capacity observing and controlling room, tin film is adhered on first cylindrical electrode and the second cylindrical electrode end face, contact sample two ends respectively again, its other end is respectively embedded into the relative both sides in retrievable capacity measurement room and flexible fastening, TT＆C system also includes Inductive component, first cylindrical electrode and the second cylindrical electrode are by anti-interference shielding line and Inductive component access Q tables.This measurement apparatus can under extreme condition under high pressure low temperature in site measurement solid insulating material dielectric dissipation factor and dielectric constant, extend existing apparatus temperature pressure and use scope, improve measurement accuracy.
Description
Technical field
The present invention relates to a kind of test device of in site measurement solid insulation material medium loss, Jie comprising insulating materials
Matter loss factor and dielectric constant, and in particular to Hydrate in Porous Medium fabricated in situ and its Jie under a kind of low temperature under high pressure
Matter is lost and dielectric constant test device.
Background technology
Gas hydrates are that one kind is formed by gas (or volatile liquid) and water under the conditions of certain temperature and pressure
Ice-like solid, be commonly called as combustible ice, be distributed widely in below the earth's surface of tundra and continental margin seabed under deposit in.My god
Right gas hydrate has huge natural gas reservoir ability, and the methane hydrate of ideal structure I types contains under 164 times of standard state
Methane gas, the gas hydrates of II type structures contain the natural gas under 184 times of standard state.Whole world gas hydrates
Reserves are very huge, and natural gas resources are 2 × 10 in estimation hydrate16m3, equivalent to 2 × 105Hundred million tons of oil equivalents, are the whole world
2 times of conventional fuel total carbon.
During the exploration and development of oil gas, geophysical method is proved to be a kind of very effective method.Electromagnetic wave
It is the new logging method grown up the eighties to propagate well logging (also known as dielectric logging), is mainly used in the dielectric constant of measurement stratum
(εr), more common has the well logging of multifrequency dielectric scanning imagery.Its principle is based on water (εr=50-80), rock (εr=5-10) and it is former
Oil (εr=2-3) the obvious difference of dielectric constant, therefore determine rock in dielectric constant, be to judge oil-bearing layer or water-bearing layer
A kind of important evidence, and this technology is widely used in pore-fluid analysis, skeleton analysis and Tectonic Analysis, over the ground
Layer is evaluated and reserves estimation.Size of the dielectric constant in rock be it is a kind of can preferably reflect the information carrier of formation physical property, from
As can be seen that dielectric constant and formation lithology, rock interior structure, especially oil gas differentiate have closely in Logging data analysis
Relation.But the current Dielectric Coefficient containing natural gas hydrate stratum is dug a well in scene, checking is counter to be pushed away the stage, well-digging
Measurement cost is high, and data acquisition interference is big.Therefore, the dielectric constant properties of gas hydrates and reservoir are studied and natural
The exploitation of the dielectric logging method of gas hydrate, has important meaning to the exploration of gas hydrates, resource assessment and exploitation
Justice, there is very big market prospects.But existing dielectric loss and dielectric constant device are mainly set at normal temperatures and pressures at present
Meter, it is impossible to meet gas hydrates and in site measurement is carried out under conditions of cryogenic high pressure.
The content of the invention
It is an object of the invention to overcome above-mentioned deficiency, there is provided one kind, the in site measurement under extreme condition under high pressure low temperature is consolidated
The dielectric dissipation factor and dielectric constant device of body insulating materials, extend the use model of existing unit temp pressure at present
Enclose, improve measurement accuracy.
To reach the purpose of foregoing invention, the present invention is achieved through the following technical solutions：
Hydrate dielectric property test device in a kind of deposit of the present invention, including it is built-in with the reaction of sample
Kettle, the air inlet/outlet of identical reaction kettle and temperature sensor on logical in succession air supply system and pumped vacuum systems, identical reaction kettle and
Data collecting system, the temperature control system of maintenance reaction kettle interior reaction temperature and the test sample dielectric that pressure transducer is electrically connected are normal
Several TT＆C systems, the TT＆C system includes the anti-interference shielding line of Q tables and coupled reaction kettle and Q tables, survey of the invention
Retrievable capacity measurement room, the first cylindrical electrode, the second cylindrical electrode and the tin film also included in reactor is put in trial assembly,
It is provided with sample carrier sheet in the middle of retrievable electric capacity observing and controlling room, is adhered on the end face of the first cylindrical electrode and the second cylindrical electrode
Contact sample two ends after tin film respectively, the other end of the first cylindrical electrode and the second cylindrical electrode is respectively embedded into retrievable electric capacity
The both sides of test cabinet, and the flexible fastening on relative wall, the Q tables of TT＆C system are electrically connected with above-mentioned retrievable capacity measurement
The first cylindrical electrode and the second cylindrical electrode of room, and it is parallel with Inductive component between Q tables and retrievable capacity measurement room.
The Q tables of the TT＆C system include electric capacity Cx test loops and inductance Lx test loops, the inductance Lx tests
After the tandem electric inductance device assembly of loop, then with electrically connecting the first cylindrical electrode or the second cylindricality electricity after the parallel connection of electric capacity Cx test loops
Pole, another electrode then accesses Q tables by anti-interference shielding line.It can realize that the resonance method solves component by Inductive component intrinsic
The interference of electric capacity, can accurately measure the dielectric loss of sample.
The two sides of the tin film is evenly coated with vaseline, and it plays adhesive attraction, and residual air between contact surface can be excluded again.
First cylindrical electrode and the second cylindrical electrode are fixed on retrievable electric capacity by spring respectively in other end
On the relative wall of test cabinet, the scalable of electrode is realized in this way, so as to ensure that electrode can fill with different-thickness sample
Tap is touched.
First cylindrical electrode and the second cylindrical electrode are cylindrical copper billet, and its end face is mirror surface structure.Mirror surface structure
It can ensure that electrode end surface is uniformly contacted with sample.
The present invention compared with prior art, has the following advantages that：
1. the present invention solves the interference of component natural capacity by the resonance method, the medium that can accurately measure sample is damaged
Consumption；
2. temperature and pressure adjustable, the dielectric loss parameter of solid sample under measurable different temperatures and pressure, is protected
Demonstrate,prove the feasibility of high pressure low temperature measurement；
3. the change of dielectric loss parameter in the measurable chemical reaction process of reactor, detects extent of reaction, can be to sample
Differential responses state is measured under the conditions of in the original location；
4. embedding extension type electrode in retrievable capacity measurement room, the dress of print is effectively ensured in retrievable capacity measurement room
Carry, extension type electrode ensures that print is fully contacted with electrode；
5. system components definite functions, with good upgradability and expandability, wide adaptability.
Brief description of the drawings
Fig. 1 is the structural representation of hydrate dielectric property test device in deposit of the invention, and wherein reactor is
The structure chart overlooked under visual angle.
Fig. 2 is the structural representation under reactor horizontal view angle in Fig. 1.
Fig. 3 is the dielectric constant at different frequencies of rock specimens containing gas hydrates.
Description of reference numerals：1- data collecting systems, 2- computers, 3- Inductive components, 4-Q tables, 5- pressure sensors, 6-
Pumped vacuum systems, 7- temperature sensors, 8- air supply systems, 9- reactors, 10- samples, 11- flexible springs, the retrievable electricity of 12-
Hold test cabinet, 13- cylindrical electrodes, 14- bolts, 15- sample carrier sheets, 16- cryogenic thermostats room, 17- reactor bottoms loop connects
Head, the anti-interference shielding lines of 18-, 19- bases, 20- end caps, 21- teflon insulation inner bags, 22- reactors, the valves of f1- first
Door, the valves of f2- second.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described with reference to the accompanying drawings and examples, shown
So, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.
The embodiment of hydrate dielectric property test device in the deposit of the present invention, referring to Fig. 1, Fig. 1 is this implementation
The structural representation of hydrate dielectric property test device in the deposit of example.Hydrate dielectric property is tested in a kind of deposit
Device includes being built-in with the reactor 22 of sample 10, the air supply system 8 of source of the gas is provided for reactor 22, pumped vacuum systems 6,
The TT＆C system of data collecting system 1, the temperature control system of the interior reaction temperature of maintenance reaction kettle 22 and test sample dielectric constant.
The reactor 22 is provided with end cap 20, and end cap 20 is connected by screw bolts with reactor 22, O-ring sealing, prevents
The inner high voltage gas leak of reactor 22.
Sample carrier sheet 15 is provided with the reactor 22, the specification of sample carrier sheet 15 is：3.5mm*3mm、φ25mm,
The sample carrier sheet 15 of the specification causes diameter phi 25mm sample to be loaded into retrievable capacity measurement room 12, refers to figure
2, the outer wall of reactor 22 is made of stainless steel, and the polytetrafluoroethylene (PTFE) for inside having insulation is made insulation inner container 21 to ensure not by stainless steel
Reactor wall electric impact, is similarly insulation and sample carrier sheet 15 and the retrievable electric capacity of polytetrafluoroethylene (PTFE) is made of polytetrafluoroethylene (PTFE)
Test cabinet 12 embeds the long 1cm of diameter phi 2cm of good conductive the first cylindrical electrode 13 and the second cylindrical electrode 23.
Require can be that sample requirement is cylinder to the section sample described in sample requirement in common test system
Shape.This is the effective way for reducing the error caused by sample edge is leaked with fringe field.Thickness of sample can 0.5-5mm it
Between, as too thin or too thick, measuring accuracy will decline, and sample is as straight as possible.Available sample is cut into slices such as rock sample,
But sample containing hydrate needs to measure under high pressure low temperature state, therefore many times can not all be difficult to ensure true sample to test.It is logical
Crossing the present invention can choose after target area core, in situ by adding high pressure low temperature condition of the natural gas of same composition in target area
Synthesis of natural gas hydrate, its capacitive properties of re-test.
Sample carrier sheet 15 is put into retrievable capacity measurement room 12, embedded the first cylindricality electricity in retrievable capacity measurement room 12
The cylindrical electrode 23 of pole 13 and second, contacts the two ends of sample 10 by tin film respectively on face at one end.The two sides of the tin film is uniform
Ground scribbles one layer of thin layer vaseline, and it plays adhesive attraction, and residual air between contact surface can be excluded again, and tin film is bonded at the first post again
On the end face of the cylindrical electrode 23 of shape electrode 13 and second.First cylindrical electrode 13 and the second cylindrical electrode 23 are cylindrical copper billet,
Its end face is mirror surface structure, and it is respectively embedded into retrievable capacity measurement room 12 in another side end face and is connected to relatively by spring
Wall on.
TT＆C system includes Q tables 4, Inductive component 3 and anti-interference shielding line 18.Q tables include three joints, two tests
Loop, i.e. electric capacity Cx test loops and inductance Lx test loops are in parallel.Inductance Lx test loops used according to frequency directly with
Electrical inductor assembly 3 is attached.Electric capacity Cx test loops used pass through reactor bottom loop by anti-interference shielding line 18
Joint 17 enters inside reactor 22, with the first cylindrical electrode 13 of corresponding retrievable capacity measurement room 12 and the second cylindricality electricity
Pole 23 is connected.
The temperature control system is cryogenic thermostat room 16, and reactor is put into cryogenic thermostat room 16 completely, followed by air bath
Ring, the temperature of maintenance reaction kettle 2 is constant.
In the present embodiment, reactor 22 passes through the first valve f1 and the second valve f2 and supply respectively provided with air inlet/outlet
System 8 is connected with pumped vacuum systems 6.In order to detect the temperature and pressure in reactor 22, apparatus of the present invention are disposed with temperature biography
The temperature test point T and the pressure monitoring point P of pressure sensor of sensor, temperature and pressure pass through temperature sensor 7 and pressure respectively
Signal is transmitted to data collecting system 1 by force snesor 5, is read by data collecting system 1 and processing data, then be transferred to computer
2 are shown and are stored.The lead of pressure sensor 5 is electrically connected with the data collecting system 1, the other end and the supply
System 8 is connected after connecting with the reactor 2；The temperature sensor 7 is inserted in the reactor kettle, temperature sensor 7
Electrically connected with the data collecting system 1.
In the present embodiment, data collecting system 1 is using the collection of Agilent company Agilent-34970A types data collecting instrument
Temperature sensor 7 and pressure sensor 5, signal are sent to computer 2 after digitizing and display is adjusted by network interface,
Computer 2 can be shown and data storage, and can complete the post processing of data.Q tables 3 use WY2358D digital display Frequency Adjustable Q tables.
Inductive component, in 0.1-1000 μ H inductance parts, is consolidated to component at different frequencies using supporting ten scopes of LK-2 for Q tables 3
There is the correction of electric capacity, the Q values and resonance value reading of reception are transferred to Q tables 3 and digital display, and record maximum Q values are harmonious automatically for Q tables 3
Value of shaking is used to calculate its dielectric dissipation factor and dielectric constant.
Sample measurement is using national standard GBT 1409-2006《Insulating material is measured in power frequency, audio, high frequency (including rice
Including ripple wavelength) under capacitivity and dielectric dissipation factor recommendation method》In the resonance method (i.e. Q tables method, test frequency scope
10kHz to 260MHz), the resonance method can be prevented effectively from equipment natural capacity by Inductive component, so as to reduce interference.Based on day
Near the frequency 100MHz at right gas hydrate exploration scene, and laboratory rebuilds gas hydrates core sample using in situ
And test.
In the present embodiment, first waterstone print 10 is loaded the print carrier sheet 15 being made up of polytetrafluoroethylene (PTFE), two
Side installs retrievable capacity measurement room 12 additional, and contacts the both sides of print 10 with cylindrical electrode 13, and retrievable capacity measurement room 12 is inserted
Enter polytetrafluoroethylene (PTFE) and insulation inner container 21 is made, connect anti-interference shielding line 18, seal up reactor end cap 20.To be residual in purging line
The interference of remaining air, opens pumped vacuum systems 6 and valve F2 starts to vacuumize system, vacuumizes and finishes after about 15 minutes, closes
The second valve F2 is closed, the first valve F1 air inlets are opened.After pressure balance, set and open constant temperature air bath 16, data acquisition
System 1, computer 2 start to monitor reaction process.Pore pressure determines by air pressure, by pressure sensor 5 and temperature sensor 7 by number
According to being transferred to data collecting system 1.The medium of rock print under the conditions of different temperature and pressures can be tested in the process
Loss situation.In the hydrate continued propagation stage, different hydrate concentration rocks can be tested under certain temperature and pressure condition
The dielectric loss and dielectric constant situation of stone print.
The present apparatus is as follows using step：
(a) normal temperature and pressure solid dielectric loss test：
In advance sample is put into reactor, then sealed.Inductive component is selected to survey according to different test frequencies after sealing
Determine Q values, calculate to determine the dielectric dissipation factor and dielectric constant of insulating materials by Q values.
(b) high pressure low temperature solid dielectric loss test：
When being related to gases at high pressure, first whole device should be hunted leak before reaction, close system exhaust valve, open air inlet
Valve then closes source of the gas, cryogenic thermostat room constant temperature closes whole reactor toward the nitrogen of injection certain pressure in reactor
One day, reactor good seal is represented if pressure gauge indicates that numerical value does not decline significantly, is if not then indicated leakage
Point, checks leak source, the presence of leak source has a strong impact on the instruction degree of accuracy of flowmeter usually using foaming agent, it is therefore necessary to strict
Close down；Nitrogen can be just bled off after leak detection, the end cap of reactor is opened, system is taken out very after adding the sample needed, good seal
Sky, then injection experimentses gas bleed off again, ensure that the air for remaining in reactor can be ignored two to three times repeatedly, finally note again
Enter to react pressure needed for air flue, one day stood after the completion of pressurization, so as to allow reaction sample, reactor pipeline and reactor wall and
Gas is allowed fully to dissolve；Constant temperature air bath allows system to be reacted, system can be carried out in the reaction to the reaction temperature of setting
Dielectric loss is tested.
The equipment is measured by the correction of reference plate at normal temperatures and pressures, and device measuring error is small, highly reliable.Height is forced down
Temperature measurement gas hydrates rock specimens result is as follows：
Fig. 3 is the dielectric constant at different frequencies of rock specimens containing gas hydrates, test temperature 273.15K and pressure
10MPa.As seen from the figure, the measurement result meets the rule that solid sample dielectric constant is reduced as frequency increases, and illustrates real
Test result effectively, demonstrate the validity that equipment is measured under high pressure low temperature.
Above-described embodiment only not limits technical scheme described in the invention to illustrate the present invention；Therefore, although
This specification is with reference to each above-mentioned embodiment to present invention has been detailed description, still, the ordinary skill of this area
Personnel should be appreciated that still can modify or equivalent substitution to the present invention；And all do not depart from the present invention spirit and
The technical scheme of scope and its improvement, it all should cover among scope of the presently claimed invention.
Claims (4)
1. hydrate dielectric property test device in a kind of deposit, including it is built-in with the reactor of sample, identical reaction kettle
Air inlet/outlet and air supply system logical in succession and pumped vacuum systems, the temperature sensor on identical reaction kettle and pressure transducer are electric
The observing and controlling system of the data collecting system of connection, the temperature control system of maintenance reaction kettle interior reaction temperature and test sample dielectric constant
System, the TT＆C system includes the anti-interference shielding line of Q tables and coupled reaction kettle and Q tables, it is characterised in that：Also include and set
In retrievable capacity measurement room, the first cylindrical electrode, the second cylindrical electrode and tin film in reactor, retrievable electric capacity observing and controlling room
Centre is provided with sample carrier sheet, and sample is contacted respectively after adhesion tin film on the end face of the first cylindrical electrode and the second cylindrical electrode
Product two ends, the other end of the first cylindrical electrode is embedded in the side of retrievable capacity measurement room, the second cylindrical electrode it is another
End face is embedded in the opposite side of retrievable capacity measurement room, and the flexible fastening on relative wall, and the Q tables of TT＆C system are electrical
Connect the first cylindrical electrode and the second cylindrical electrode of above-mentioned retrievable capacity measurement room, and Q tables and retrievable capacity measurement room
Between be parallel with Inductive component；First cylindrical electrode is fixed on retrievable capacity measurement room one in other end by spring
On individual wall, second cylindrical electrode is fixed on relative another in retrievable capacity measurement room in other end by spring
On wall.
2. hydrate dielectric property test device in deposit according to claim 1, it is characterised in that：The observing and controlling system
The Q tables of system include electric capacity Cx test loops and inductance Lx test loops, the inductance Lx test loops tandem electric inductance device assembly
Afterwards, then after in parallel with electric capacity Cx test loops the first cylindrical electrode or the second cylindrical electrode are electrically connected, another electrode then passes through
Anti-interference shielding line accesses Q tables.
3. hydrate dielectric property test device in deposit according to claim 1, it is characterised in that：The tin film
Two sides is evenly coated with vaseline.
4. hydrate dielectric property test device in deposit according to claim 1, it is characterised in that：First post
Shape electrode and the second cylindrical electrode are cylindrical copper billet, and its end face is mirror surface structure.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410722729.XA CN104407233B (en) | 2014-12-02 | 2014-12-02 | Hydrate dielectric property test device in a kind of deposit |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410722729.XA CN104407233B (en) | 2014-12-02 | 2014-12-02 | Hydrate dielectric property test device in a kind of deposit |
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| CN104407233A CN104407233A (en) | 2015-03-11 |
| CN104407233B true CN104407233B (en) | 2017-10-27 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10883952B2 (en) * | 2015-10-15 | 2021-01-05 | Shiraishi Kogyo Kaisha, Ltd. | Method for calculating dielectric constant of particle-dispersed composite materials and method for evaluating dispersibility |
| CN109581159B (en) * | 2018-11-30 | 2020-01-21 | 华北电力大学 | Insulating liquid state, gaseous state and gas-liquid mixture state dielectric property test chamber |
| CN110133061B (en) * | 2019-05-17 | 2020-06-16 | 中国科学院化学研究所 | High-temperature sample table suitable for testing dielectric property of material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1065478A1 (en) * | 1999-07-02 | 2001-01-03 | Institut Francais Du Petrole | Capacitive detector for measuring the level of an electric conductive liquid in a container and method for manufacturing such a detector |
| CN101329375A (en) * | 2008-07-29 | 2008-12-24 | 中国科学院物理研究所 | Device and method for measuring dielectric constant and dielectric loss of sample under low temperature and high voltage |
-
2014
- 2014-12-02 CN CN201410722729.XA patent/CN104407233B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1065478A1 (en) * | 1999-07-02 | 2001-01-03 | Institut Francais Du Petrole | Capacitive detector for measuring the level of an electric conductive liquid in a container and method for manufacturing such a detector |
| CN101329375A (en) * | 2008-07-29 | 2008-12-24 | 中国科学院物理研究所 | Device and method for measuring dielectric constant and dielectric loss of sample under low temperature and high voltage |
Non-Patent Citations (2)
| Title |
|---|
| 含天然气水合物的海底沉积物的电学特性实验;陈玉凤等;《地球物理学进展》;20130430;第28卷(第2期);文章第1042页右栏第3段-第1044页右栏第1段，图1 * |
| 温度周期变化下分散型天然气水合物的沉积物电阻率测量;陈玉凤等;《海洋地质前沿》;20130731;第29卷(第7期);文章第20页左栏第2段-第21页左栏倒数第1段，图4-5 * |
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