CN103116077A - Device for in site measurement of hydrate sediment resistivity - Google Patents
Device for in site measurement of hydrate sediment resistivity Download PDFInfo
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- CN103116077A CN103116077A CN2013100183277A CN201310018327A CN103116077A CN 103116077 A CN103116077 A CN 103116077A CN 2013100183277 A CN2013100183277 A CN 2013100183277A CN 201310018327 A CN201310018327 A CN 201310018327A CN 103116077 A CN103116077 A CN 103116077A
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Abstract
The invention discloses a device for in site measurement of hydrate sediment resistivity. The device for the in site measurement of the hydrate sediment resistivity comprises a hydrate reaction kettle, a gas cylinder and a vacuum pump, wherein a temperature sensor and a pressure sensor are respectively arranged in the hydrate reaction kettle, a constant temperature test box is arranged on the periphery of the hydrate reaction kettle, the vacuum pump is connected with an input pipeline, a first stop valve and a second stop valve are arranged on the input pipeline in sequence, the input pipeline is input in the reaction kettle, a vacuum manometer and a manifold pressure gauge are further arranged on the vacuum pump, the gas cylinder is connected to the input pipeline between the first stop valve and the second stop valve through a third stop valve, the other ends of the temperature sensor and the pressure sensor are respectively connected to data acquisition instruments, the bottom end of the hydrate reaction kettle is connected to the data acquisition instruments respectively through a digital alternating current bridge and an information processing system. According to a unique design of hydrate formation setting, formation of different types and amounts of hydrate is fulfilled, especially synthesis of the hydrate in sediments.
Description
Technical field
The present invention relates to a kind of in site measurement hydrate or contain the device of the sedimental resistivity of hydrate.
Background technology
Gas hydrate is a kind of ice shape crystal class compound that one or more gases or volatile liquid and water generate under uniform temperature and pressure.Exist a large amount of natural gas hydrate resources (principal ingredient is methane gas and water) on the earth, it mainly composes unconsolidated sediment and the permafrost that is stored in following 0～1500 meter of seabed.Natural gas hydrate resources is considered to the promising new forms of energy of a kind of richness.Containing the hydrate saturation degree is an important parameter of natural gas hydrate resources estimation.At present, resistivity logging is that definite hydrate is composed one of effective ways of depositing position and estimation hydrate concentration.Hydrate is a kind of intimate insulator.When hydrate formed in the sediment hole, the sedimental resistivity that contains hydrate can be higher than water saturated sedimental resistivity.Therefore, to contain the sedimental electrology characteristic of gas hydrate all significant to the estimation of the reservoirs exploration of gas hydrate and reserves in research.
Due to high well logging expense, the complexity of sea bed gas hydrate is composed environment and the gas hydrate instability at normal temperatures and pressures of depositing, and the electrology characteristic that modeling effort contains the gas hydrate marine bottom sediment is a kind of important means.At present, the resistivity data about the marine bottom sediment that contains gas hydrate lacks.People are general adopts the main electrode catheter method of constant current-supplying that adopts to measure carbon dioxide or Tetrahydrofuran hydrate sample.There is the deficiency of following two aspects in this measuring method: on the one hand, the formation condition of carbon dioxide or Tetrahydrofuran hydrate is simpler, but the occurrence condition of its formed hydrate sample and natural sea bed gas hydrate and characteristic make a big difference.On the other hand, due to the unevenness of electrode system peripheral region hydrate, and solution easily produces electric polarization and electrochemical reaction under constant current, and therefore, the measurement result that obtains can be very untrue.
Summary of the invention
The object of the invention is to overcome the deficiency of above-mentioned hydrate method of measuring resistivity, provide a kind of can the in site measurement hydrate or contain the method and apparatus of hydrate sediment resistivity, provide important referential data for studying the actual sedimental saturation degree research of sea bed gas hydrate.
For realizing above purpose, the present invention has taked following technical scheme: a kind of in site measurement contains the device of the sedimental resistivity of hydrate, comprise hydrate reaction still, gas cylinder, vacuum pump, be respectively equipped with temperature sensor and pressure transducer in described hydrate reaction still, the hydrate reaction still is arranged with Homothermal Proof Box outward; Vacuum pump is connected with intake line, be provided with successively the first stop valve, the second stop valve on this intake line, intake line is input in reactor, also be provided with corresponding pressure vacuum gauge and boost gauge on this intake line, described gas cylinder is connected on intake line between the first stop valve and the second stop valve by the 3rd stop valve; Described temperature sensor and the pressure transducer other end are connected respectively to data collecting instrument, and the bottom of described hydrate reaction still is connected to data collecting instrument by Digital AC electric bridge and information handling system respectively.
Described hydrate reaction still comprises blind flange and the stainless steel kettle that is bolted, and has pressure tap, temperature-measuring port, air intake opening on blind flange, and pressure tap is connected correspondence and is connected with pressure transducer with temperature sensor with temperature-measuring port; Stainless steel kettle inboard is provided with polytetrafluoroethyllining lining, establishes the copper billet electrode on polytetrafluoroethyllining lining, and the copper billet electrode is connected with the electric wire outlet that is located at stainless steel kettle bottom, also is provided with the teflon orifice plate between the copper billet electrode.
The hydrate reaction still as shown in fig. 1, it is to be placed in Homothermal Proof Box.This reactor comprises the reactor main body cylindraceous of upper end open, is arranged on the upper flange lid of reactor body openings end, is arranged on upper flange lid air intake opening, pressure tap and temperature-measuring port, is placed on reaction kettle body teflon inner core side copper billet electrode.Be placed on the teflon orifice plate of inner core side, gas is diffused in the sediment hole by the hole of orifice plate, promotes the generation of hydrate in sediment.Be arranged on the contact conductor outlet of reactor bottom part body, this exit is clamped external wire by two shells and is connected with alternating current bridge.The beasurement base of resistivity is:
Wherein r is the resistivity of hydrate or hydrate sediment, Ω .m; R is the resistance of hydrate or hydrate sediment, Ω; L is the length of the sample between the copper billet electrode, m; A is the copper billet electrode area that contacts with sample, m
2The power supply mode of resistance measurement has constant current source and constant pressure source.This place adopts alternating current bridge to measure the rectangular-shaped hydrate between the copper billet electrode or contain the sedimental resistance R of hydrate.This resistivity measurement mode reduces electrode polarization and electrochemical reaction, has not only improved the accuracy of resistivity measurement, has also realized hydrate or has contained the sedimental resistivity in site measurement of hydrate.
The observing and controlling acquisition system is by temperature, pressure, and resistance measuring system and data collecting instrument and computer form, and can gather the temperature of coming, pressure, the measurement data of resistance is processed, tracking reaction process.
The using method of native system is as follows: reacting gas is entered into the reactor that is immersed in temperature-controlling system by gas handling system, with other reactants in still water generation reaction compound or contain the hydrate sediment sample under certain temperature and pressure, wherein temperature conditions is controlled by temperature-controlling system, and by the observing and controlling acquisition system, the real-time measurement of the gas hydrate that reaction is generated or the resistivity physical property of hydrate sediment.Before air inlet, first reaction liquid or sediment are injected reactor 4, then fastening upper flange lid 4-1 vacuumizes.Temperature is adjusted to required temperature conditions, the beginning air inlet, and open the observing and controlling acquisition system, namely cocoa carries out in real time sample, in site measurement.Therefore this process comprises two aspects:
1) hydrate or the hydrate reaction of formation in sediment.The temperature, pressure design of this experimental provision can generate polytype gas hydrate;
2) resistivity physical property measurement.This place method of measuring resistivity can be rapidly to the hydrated in-situ thing or contain the resistivity original position of hydrate sediment sample, in real time, Measurement accuracy native system temperature measurement range :-20～50 ℃, maximum working pressure (MWP) is 20Mpa, and institute's measuring resistance rate scope is 1.7*10
-8Ω .m～1*10
12Ω .m.
The present invention compared with prior art has following advantage:
1. unique hydrate generates the design that arranges and can satisfy the hydrate of dissimilar and different amounts and synthesize, particularly synthesizing in sediment.
2. realize to the resistivity of hydrated in-situ thing in real time, measure accurately.
3. can carry out to the core sample of sampling on the spot pressurize, insulation measurement, judge that further the position is deposited in the tax of sea bottom hydrate.
4. by corresponding software, coordinate the measurement of resistivity data to determine the approximate content of hydrate in institute's sample thief on the spot, thereby these regional hydrate reserves are estimated.
5. also can measure the resistivity of the harsher material of some conditions, especially low temperature, under high pressure.
6. adopted the integration design, compact conformation.
Description of drawings
Fig. 1 is the structural representation that whole hydrate generates proving installation;
Fig. 2 is the inner structure schematic diagram of hydrate reaction still;
Fig. 3 is in Fig. 2, the vertical view of tetrafluoroethene orifice plate and copper billet electrode.
Embodiment
Below in conjunction with the drawings and specific embodiments, content of the present invention is described in further details.
Designed an experimental provision by Fig. 1, Fig. 2 and Fig. 3, except specifying, all connecting tubes are that external diameter is the stainless-steel tube of 3mm, and use is threaded, the sealing of snap ring cutting ferrule.The urceolus material of reactor is 1Cr18Ni9Ti, and liner is corrosion resistant teflon.The upper flange lid is bolted kettle and the sealing of O RunddichtringO.The withstand voltage 20Mpa of reactor, high 115cm, kettle wall thickness 25cm, the thick 20cm of liner.Kettle height 95cm.The maximum volume of reactor is 85ml.Two copper electrode symmetries are positioned over inner core.Copper wire passes liner and draws from the kettle lower end.
a kind of in site measurement contains the device of the sedimental resistivity of hydrate, comprise hydrate reaction still 4, gas cylinder 11, vacuum pump 1, be respectively equipped with temperature sensor 2 and pressure transducer 6 in hydrate reaction still 4, the outer Homothermal Proof Box 3 that is arranged with of hydrate reaction still 4, air supply system comprises vacuum pump 1, high pressure methane gas cylinder 11, stop valve the second stop valve 5, stop valve 7, the first stop valve 14, boost gauge 15, pressure vacuum gauge 13, the major function of this system is to realize the circulation of gas and the detection of gas state parameter, high pressure methane gas cylinder 11 provides the methane gas of high pressure, using vacuum pump 1 before hydrate reaction takes out in most still and the residual air of pipeline, need before reaction all valve opens, open fast continuously the 3rd stop valve 12, squeeze portion of air thereby allow gas in gas cylinder wash away continuously pipeline, after this close the 3rd valve 12, open vacuum pump and begin to vacuumize.After whole system is exhausted vacuum, close the first valve 14, open the 3rd valve 12 beginning air inlets; Vacuum pump 1 is connected with intake line, be provided with successively the first stop valve 14, the second stop valve 5 on this intake line, intake line is input in reactor 4, also be provided with corresponding pressure vacuum gauge 13 and boost gauge 15 on this intake line, gas cylinder 11 is connected on intake line between the first stop valve 14 and the second stop valve 5 by the 3rd stop valve 12; Temperature sensor 2 and pressure transducer 6 other ends are connected respectively to data collecting instrument 10, and the bottom of hydrate reaction still 4 is connected to data collecting instrument 10 by Digital AC electric bridge 8 and information handling system 9 respectively.
Temperature-controlling system comprises Homothermal Proof Box 3, and the model of this constant temperature oven is the Challenge250 microthermal climate chamber of ACS company.The reaction that can be hydrate provides required temperature conditions.
The structure of hydrate reaction still as shown in Figure 2, the vertical view of copper billet electrode and teflon orifice plate is as shown in Figure 3.4-1 is the upper flange lid, and it is connected with reaction kettle body by bolt, and adopts double-deck O type fluorine rubber sealing; 4-2 is the copper billet electrode that is positioned over the liner side; The copper billet electrode is semi-cylindrical, and its floorage is 10.5cm
2, be highly 3.5cm, width is 3.47cm.4-3 is for bearing the stainless steel kettle of high pressure; 4-4 is corrosion resistant polytetrafluoroethyllining lining; 4-5 is connecting copper block and passes the copper wire that liner is drawn from the bottom; 4-6 is pressure tap, and it can connect to measure the gaseous tension pressure transducer in reactor; 4-7 is temperature-measuring port, and it can connect to measure sample temperature temperature sensor in reactor; 4-8 is air intake opening.These 3 outlets all are threaded connection, the sealing of snap ring cutting ferrule.4-9 is the nylon drum pressure, is used for sealing copper wire, guarantees that under high pressure, gas can not leak out from the electrode wires outlet; 4-10 is the electric wire outlet, clamps external wire by two shells and is connected with alternating current bridge; 4-11 is bolt, is used for connecting sealing flange cover and kettle; 4-12 is the teflon rectangle orifice plate that is placed on the liner another side.Its length is 2.5cm, and width is 3.0cm, and thick is 0.5cm, and small sircle hole is arranged on plate, and gas can diffuse to sample by circular hole, promotes the formation of hydrate in hole.The formed hydrate sample of this covering device is rectangular-shaped, and the amount of sample is not subjected to the restriction of reactor volume.
The observing and controlling acquisition system comprises for the temperature sensor 2 of measuring sample temperature, pressure transducer 6, and Digital AC electric bridge 8 and data collecting instrument 10 and computer 9 form.Data collecting instrument is the Agilent34901A data acquisition system (DAS) of being made by U.S. Agilent company.
Embodiment one:
In Fig. 1,2 and 3, come the synthesizing methane hydrate with methane gas and pure water.With pure water cleaning reaction still 4, then add the pure water of 25 grams, cover upper flange lid 4-1 sealing.The 3rd stop valve 12 is opened, squeezed portion of air thereby allow methane gas in gas cylinder 11 wash away continuously pipeline, after this close the 3rd stop valve 12, open the first stop valve 14, open vacuum pump, the air in pipeline and still is taken away.After vacuum meter is stable, close the first stop valve 14, open the 3rd stop valve 12 beginning air inlets, after system pressure is stable, stop air inlet.The pressure of methane that this reaction is used is 10Mpa.Then opening Homothermal Proof Box 3, is 0 ℃ with the Temperature Setting that reacts.And open the observing and controlling acquisition system, carry out pressure, displacement, temperature, the collection of resistance signal.
Methane enters in reactor 4 by the air intake opening 4-8 on hydrate reaction still 4, and through certain induction time, the water in methane and still reacts.Etc. (temperature, pressure no longer changes) after complete reaction, continued to keep reaction temperature, pressure parameter used 2～3 days, guarantee the aging of sample.Finish subsequently experiments of measuring.The result demonstration, the electrical resistivity range of methane hydrate sample is 11.6*10
-3Ω .m-5*10
3Ω .m, experimental result shows, and this device can form hydrate preferably, and measuring method used is the synthesizing methane hydrate preferably, and measuring method used can be completed the in site measurement to the resistivity of hydrate well.
Embodiment two:
With 3.5% sodium chloride solution, the synthetic gas hydrate that are filled in the porous medium hole of 60～100 purpose silica sands and methane more.This example is the resistivity measurement of simulated sea bottom gas hydrate sediment sample.
At first screen 60～100 purpose silica sands, clean up, put into reactor 4, add simultaneously 3.5% sodium chloride solution, make sand grains reach certain saturated.Open vacuum pump 1, vacuumize to remove the gas in reactor 4, then pass into required methane gas, make pressure reach hydrate and generate required reaction pressure, close gas admittance valve.Place after a while, make methane gas fully water-soluble.Then the Temperature Setting of adjusting Homothermal Proof Box 3 is 2 ℃, beginning synthesized hydrate in sediment.Etc. (temperature, pressure no longer changes) after complete reaction, continued to keep reaction temperature, pressure parameter used 2～3 days, finish subsequently experiments of measuring.The turn-on data acquisition system records the temperature in whole hydrate formation, pressure, and the measurement variation situation of resistance, result shows: the sedimental electrical resistivity range of the gas hydrate that generate is 1.5 Ω .m-5 Ω .m.Experiment showed, that this device can measure the resistivity of porous medium hydrate preferably.
After test finishes, coordinate corresponding computer software to ask the content of Hydrate in Porous Medium.This software is based on the Archie equation that the gas hydrate resistivity logging uses and uses Visual Basic language establishment, the hypothesis hydrate is equally distributed in model, by Archie equation, to the result of calculation of example 2 be: the saturation degree of gas hydrate is 15%.This result is compared with the sedimental saturation degree of nature sea bed gas hydrate, and is still more rational.This proves that this device coordinates corresponding software can estimate hydrate content in sample.
Above-listed detailed description is that this embodiment limits the scope of the claims of the present invention for the illustrating of possible embodiments of the present invention, and the equivalence that all the present invention of disengaging do is implemented or change, all should be contained in the scope of the claims of this case.
Claims (2)
1. an in site measurement contains the device of the sedimental resistivity of hydrate, it is characterized in that: comprise hydrate reaction still (4), gas cylinder (11), vacuum pump (1), be respectively equipped with temperature sensor (2) and pressure transducer (6) in described hydrate reaction still (4), the outer Homothermal Proof Box (3) that is arranged with of hydrate reaction still (4);
Vacuum pump (1) is connected with intake line, be provided with successively the first stop valve (14), the second stop valve (5) on this intake line, intake line is input in reactor (4), also be provided with corresponding pressure vacuum gauge (13) and boost gauge (15) on this intake line, described gas cylinder (11) is connected on intake line between the first stop valve (14) and the second stop valve (5) by the 3rd stop valve (12);
Described temperature sensor (2) and pressure transducer (6) other end are connected respectively to data collecting instrument (10), and the bottom of described hydrate reaction still (4) is connected to data collecting instrument (10) by Digital AC electric bridge (8) and information handling system (9) respectively.
2. in site measurement as claimed in claim 1 contains the device of the sedimental resistivity of hydrate, it is characterized in that: described hydrate reaction still (4) comprises blind flange (4-1) and the stainless steel kettle (4-3) that connects by bolt (4-11), have pressure tap (4-6), temperature-measuring port (4-7), air intake opening (4-8) on blind flange (4-1), pressure tap (4-6) is connected 4-7 with temperature-measuring port) correspondingly respectively be connected 6 with temperature sensor (2) with pressure transducer) be connected; Stainless steel kettle (4-3) inboard is provided with polytetrafluoroethyllining lining (4-4), establish copper billet electrode (4-2) on polytetrafluoroethyllining lining (4-4), copper billet electrode (4-2) is connected with the electric wire outlet (4-10) that is located at stainless steel kettle (4-3) bottom, also is provided with teflon orifice plate (4-12) between copper billet electrode (4-2).
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Cited By (8)
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| CN103604996A (en) * | 2013-11-28 | 2014-02-26 | 国家电网公司 | Device and method for measuring overhead stranded wire resistance temperature coefficient |
| CN105004837A (en) * | 2015-06-26 | 2015-10-28 | 中国科学院力学研究所 | Natural gas hydrate sediment multi-measurement unit analysis method and integrated system |
| CN105136862A (en) * | 2015-08-25 | 2015-12-09 | 西南石油大学 | Measuring device for natural gas hydrate reaction rate |
| CN108169050A (en) * | 2017-12-28 | 2018-06-15 | 黑龙江科技大学 | A kind of Gas Hydrate saturation degree monitoring device |
| CN108445189A (en) * | 2018-04-27 | 2018-08-24 | 青岛海洋地质研究所 | The quiet spy parameter simulation device of engineering containing hydrate sediment and method |
| CN110068733A (en) * | 2019-05-21 | 2019-07-30 | 中国科学院地质与地球物理研究所 | A kind of device and method measuring gas hydrates coring drilling with keep up pressure sample resistivity |
| CN110672667A (en) * | 2019-10-17 | 2020-01-10 | 北京航空航天大学 | Dynamic piezoresistive probe for measuring plasma deposition |
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| CN103604996A (en) * | 2013-11-28 | 2014-02-26 | 国家电网公司 | Device and method for measuring overhead stranded wire resistance temperature coefficient |
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| CN110068733A (en) * | 2019-05-21 | 2019-07-30 | 中国科学院地质与地球物理研究所 | A kind of device and method measuring gas hydrates coring drilling with keep up pressure sample resistivity |
| CN110068733B (en) * | 2019-05-21 | 2020-03-27 | 中国科学院地质与地球物理研究所 | Device and method for measuring resistivity of natural gas hydrate pressure-maintaining coring sample |
| CN110672667A (en) * | 2019-10-17 | 2020-01-10 | 北京航空航天大学 | Dynamic piezoresistive probe for measuring plasma deposition |
| CN110672667B (en) * | 2019-10-17 | 2021-02-26 | 北京航空航天大学 | Dynamic piezoresistive probe for measuring plasma deposition |
| CN110967769A (en) * | 2019-12-11 | 2020-04-07 | 中国地质科学院地球物理地球化学勘查研究所 | Online observation device and online observation method for hydrate rock core |
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Application publication date: 20130522 |