CN115406939B - Electrical parameter detection and treatment system and method for loose deposit containing hydrate - Google Patents

Electrical parameter detection and treatment system and method for loose deposit containing hydrate Download PDF

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CN115406939B
CN115406939B CN202110589809.2A CN202110589809A CN115406939B CN 115406939 B CN115406939 B CN 115406939B CN 202110589809 A CN202110589809 A CN 202110589809A CN 115406939 B CN115406939 B CN 115406939B
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CN115406939A (en
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魏伟
邢兰昌
张树立
王斌
韩维峰
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Petrochina Co Ltd
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
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Abstract

The invention provides an electrical parameter detection and treatment system and method for loose sediment of hydrate, wherein the system comprises a sample holder and a parameter detection and treatment device; the sample holder is used for holding a cylindrical sample to be measured containing loose hydrate sediment; the parameter detection and processing device comprises a first electrode system, a second electrode system, a first multi-path switching module, a second multi-path switching module, a signal excitation module, a first data acquisition module, a second data acquisition module, a first current measurement module, a second current measurement module, a voltage measurement module and a controller; the first electrode system and the second electrode system are respectively arranged on two end surfaces of the sample in a contact manner and are concentric ring disk electrodes, the concentric ring disk electrodes comprise a central disk electrode and at least one ring electrode, and the ring electrodes are sleeved outside the disk electrode and the ring electrodes in sequence from small to large in size; and electric insulation materials are arranged between the disc electrode and the annular electrode and between the annular electrode and the annular electrode.

Description

Electrical parameter detection and treatment system and method for loose deposit containing hydrate
Technical Field
The invention relates to an electrical parameter detection and treatment system and method for loose sediment containing hydrate, and belongs to the technical field of natural gas hydrate exploration and development.
Background
The natural gas hydrate is a novel clean energy source with huge reserves and high energy density, and the qualitative identification and the fine quantitative evaluation technology of the natural gas hydrate reservoir are key to restrict accurate estimation of the hydrate resource amount. Currently, the art generally adopts geophysical methods to explore hydrates, wherein the physical properties of a hydrate-containing reservoir, accurate acquisition of physical parameters, and establishment of quantitative relationships between physical parameters and reservoir properties are the basis for developing novel hydrate exploration and evaluation techniques.
In order to obtain physical parameters of the hydrate-containing sediment, in particular, electrical characteristic parameters (electrical parameters), such as resistivity, complex resistivity and the like, a rock physical simulation experiment is usually carried out, a reaction container and a matched assembly capable of simulating the occurrence environment condition of the hydrate are required to be designed, and then an electrical parameter test system, a test method and a data processing method are developed.
It is common in the art to mount a pair of parallel electrode plates to two parallel end faces of a cylindrical sample of loose deposit of hydrate, and to test the sample using resistance or impedance measurements. The resistivity or complex resistivity of the hydrate-containing sediment sample is calculated by using the measured resistance or impedance data in combination with the geometry of the sample, ignoring the anisotropy of the sample. However, such techniques suffer from the drawbacks:
(1) Data measurement: the electrode plate is in poor contact with the hydrate loose deposit, and an interface with variable magnitude and characteristics is generated between the electrode plate and the hydrate loose deposit, so that the test data not only comprises the electrical characteristics of the sample to be tested, but also comprises interface resistance or interface impedance of the interface. Thus, current data measurement techniques suffer from the disadvantage that raw measurement data reflecting the electrical properties of the hydrate-containing bulk sediment sample is not truly obtained.
(2) And (3) data processing: according to analysis, the interface resistance or interface impedance is influenced by various factors, such as test signal frequency, test signal waveform, test signal amplitude, sediment compactness, pore water salt ion concentration and the like, and the various influencing factors lead to extremely limited applicability of the current data processing methods, such as a theoretical analysis method, an equivalent circuit method and the like, and only qualitative analysis results can be given, but accurate electrical characteristic parameters, such as resistivity, complex resistivity and the like, of a special tested object, such as loose sediment containing hydrate cannot be obtained quantitatively.
Therefore, it has become a technical problem to be solved in the art to provide a novel electrical parameter detection and processing system and method that can accurately measure loose deposits containing hydrates (natural gas hydrates).
Disclosure of Invention
To address the above-described shortcomings and drawbacks, it is an object of the present invention to provide an electrical parameter detection and treatment system for loose deposits of aqueous compounds.
It is also an object of the present invention to provide a method for detecting and treating electrical parameters of loose deposits of hydrate.
To achieve the above object, in one aspect, the present invention provides an electrical parameter detection and treatment system for loose deposits of hydrate, wherein the system comprises: the device comprises a sample holder and a parameter detection and processing device, wherein the sample holder is used for holding a sample to be detected of loose sediment of a hydrate, and the sample is cylindrical; the parameter detection and processing device comprises a first electrode system, a second electrode system, a first multipath switching module, a second multipath switching module, a signal excitation module, a first data acquisition module, a second data acquisition module, a first current measurement module, a second current measurement module, a voltage measurement module and a controller;
The first electrode system and the second electrode system are respectively arranged at two end surfaces of the cylindrical sample in a contact manner, the first electrode system and the second electrode system are concentric ring disk electrodes, the concentric ring disk electrodes comprise a central disk electrode and at least one ring electrode, and the ring electrodes are sleeved outside the disk electrode and the ring electrode in the sequence from small to large in size; the gaps between the disc electrode and the annular electrode and between the annular electrode and the annular electrode are provided with electric insulation materials;
The controller is electrically connected with the first multi-path switching module through the signal excitation module, the first multi-path switching module is electrically connected with the first electrode system and the second electrode system through the first current measuring module and the second current measuring module through leads respectively, the first electrode system and the second electrode system are also electrically connected with the controller through the second multi-path switching module, the voltage measuring module and the second data acquisition module, the first current measuring module and the second current measuring module are electrically connected with the controller through the first data acquisition module and the second data acquisition module respectively, and the first multi-path switching module and the second multi-path switching module are electrically connected with the controller respectively.
As a specific embodiment of the system of the present invention, the first multi-path switching module is electrically connected to the two concentric ring plate electrode assemblies (i.e. the first electrode assembly and the second electrode assembly) through the first current measurement module and the second current measurement module respectively, and the two concentric ring plate electrode assemblies are electrically connected to the controller through the second multi-path switching module, the voltage measurement module and the second data acquisition module respectively;
In addition, the first multi-path switching module can be electrically connected with the disc electrode and the annular electrode in the two concentric ring disc electrodes (namely the first electrode system and the second electrode system) through the first current measuring module and the second current measuring module respectively through leads, and the disc electrode and the annular electrode in the two concentric ring disc electrodes are electrically connected with the controller through the second multi-path switching module, the voltage measuring module and the second data acquisition module.
As a specific embodiment of the system of the present invention, the number of the ring-shaped electrodes is 1-3.
As a specific embodiment of the above system of the present invention, the leads may be soldered to the corresponding electrodes.
As a specific embodiment of the system of the present invention, the sample holder includes a holder body and ends detachably connected to two ends of the holder body; the end head is provided with a lead wire guide pipe for leading a lead wire connected with the electrode out of the sample holder;
The clamp holder body comprises a rubber sleeve, an inner shell and an outer shell, wherein the inner shell and the outer shell are cylindrical, and the outer shell is sleeved outside the inner shell and forms a first gap between the outer shell and the inner shell (namely, a jacket structure is formed between the inner shell and the outer shell);
the rubber sleeve is used for fixing (wrapping) a sample to be tested of the hydrate loose sediment, the rubber sleeve is positioned in the inner shell, and a second gap is reserved between the rubber sleeve and the inner shell.
As a specific embodiment of the system of the present invention, the inner casing and the outer casing are respectively provided with a confining pressure fluid opening and a cooling liquid opening, and the confining pressure fluid opening and the cooling liquid opening are respectively connected with the confining pressure fluid tank and the constant temperature water tank through a confining pressure fluid conduit and a cooling liquid conduit by a confining pressure pump and a cooling circulating pump so as to respectively introduce confining pressure fluid and cooling liquid into the second gap and the first gap;
The inner shell, the outer shell and the rubber sleeve are correspondingly provided with a vacuumizing port and an injection port, and the vacuumizing port is connected with a vacuum pump through a vacuum conduit; the injection port is connected with a gas bottle or a liquid bottle through a gas injection or water injection conduit and a booster pump or a liquid injection pump.
As a specific embodiment of the system of the present invention, the sample holder is further provided with a plurality of pressure sensors and a plurality of temperature sensors for measuring the temperature of the cooling liquid, the confining pressure, the pressure and the temperature in the sample to be measured.
As a specific embodiment of the system according to the present invention, the rubber sleeve is made of buna rubber or fluororubber.
In a specific embodiment of the system according to the present invention, the inner housing, the outer housing and the end are made of stainless steel, and the stainless steel includes type 304, type 316 or type 316L stainless steel.
As a specific embodiment of the system according to the present invention, the width of the first gap is 2cm.
In the invention, the multipath switching module, the signal excitation module, the data acquisition module, the current measurement module, the voltage measurement module and the controller are all conventional devices; for example, in a specific embodiment of the present invention, the controller may be a computer with measurement and control software (conventional software) installed therein, for performing parameter configuration and operation mode control on the multi-channel switching module, the signal excitation module, and the data acquisition module, and after acquiring data from the data acquisition module, performing analysis processing on the data by using the conventional measurement and control software installed therein;
the multi-path switching module is used for realizing the purpose of communicating the needed electrodes by switching the states of opening and closing a plurality of switches in the module;
the signal excitation module provides excitation signals required for measuring electrical parameters, such as sine wave signals with certain amplitude and initial phases;
The data acquisition module synchronously acquires an excitation signal and a signal passing through the electrode and the sample to be detected; in an embodiment of the present invention, the data acquisition module may be, for example, a data acquisition card;
The current measuring module and the voltage measuring module are respectively used for measuring the current and the voltage applied to the sample to be measured.
In the invention, the system also comprises a power supply for providing electric energy for each device, and can also comprise a flowmeter, a metering pump and the like for metering and leading out gas and aqueous solution from a sample to be tested according to requirements.
In another aspect, the invention also provides a method for detecting and treating electrical parameters of loose deposit of hydrate, wherein the method comprises the following steps:
(1) Placing a sample to be tested of the hydrate-containing loose deposit into a sample holder, or placing raw material components for preparing the sample to be tested of the hydrate-containing loose deposit into the sample holder and preparing the sample to be tested;
(2) According to the required detection conditions, working parameters of a signal excitation module, a multi-path switching module and a data acquisition module are configured;
(3) Two concentric ring disk electrodes form electrode pairs, and the electrical parameters of the whole sample under different excitation signal frequencies are respectively measured; respectively adopting two concentric ring disk electrodes to measure the electrical parameters of the interface between the electrode and the sample to be measured under different excitation signal frequencies;
(4) Measuring the current and the voltage passing through the sample to be measured from the corresponding measuring electrode by a current measuring module and a voltage measuring module;
(5) And (3) collecting the current and voltage data obtained in the step (4) by using a data collection module, and then processing the current and voltage data to obtain the electrical parameters of the sample to be tested.
In the invention, a sample to be tested containing the loose deposit of the hydrate can be formed in a sample holder, or can be placed in the sample holder after being generated outside the sample holder; correspondingly, the invention can implement static measurement of the electrical parameters of the sample to be measured, namely, the state of the sample to be measured is kept unchanged, and the electrical parameters of the sample to be measured are measured; the invention can also be used for dynamically measuring the electrical parameters of the sample to be measured, namely, the electrical parameters of the sample to be measured are measured in the state change process of the sample to be measured, such as the gradual generation process of hydrate in simulated sediment or the gradual decomposition process of the hydrate, and the information of the dynamic change of the electrical parameters of the sample to be measured along with time is obtained by measurement. In this case, the static measurement can be regarded as a special case of the dynamic measurement, so that the invention is described in the context of a dynamic measurement process, which is equally applicable to the static measurement.
As a specific embodiment of the above method of the present invention, in the step (1), the preparation of the sample to be tested for the loose deposit of the hydrate comprises the following specific steps:
1) Opening a sample holder, and adding raw material components for preparing a sample to be tested of the loose deposit of the hydrate into a rubber sleeve of the sample holder; the raw material components comprise natural sea sand and/or quartz sand;
2) After all parts of the sample holder are assembled, the raw material components are vacuumized by utilizing a vacuum pump, then a booster pump and a liquid injection pump are started to charge water solution and gas with certain salinity into the raw material components, then a confining pressure pump is started to apply confining pressure to the sample, and a cooling circulating pump and a constant-temperature water tank are started to cool the sample and keep a constant-temperature environment.
As a specific embodiment of the above method of the present invention, typical working conditions include: the confining pressure was 10MPa, the pore pressure in the simulated deposit was 8MPa, and the cooling water temperature was 1 ℃. Wherein, confining pressure and cooling liquid (water) temperature are used for ensuring that experimental conditions can simulate field environment.
In the invention, the raw material components for preparing the sample to be tested of the hydrate loose sediment mainly comprise simulated sediment with different particle sizes, such as natural sea sand and/or quartz sand.
As a specific embodiment of the above method of the present invention, wherein the feedstock component further comprises kaolin to simulate clay composition in the deposit.
As a specific embodiment of the method, the gas is methane, and the aqueous solution with certain salinity is NaCl aqueous solution with mass fraction of 3.5%.
The injection sequence of the aqueous solution with certain salinity and the gas is not particularly required, and the raw material components are firstly filled with the aqueous solution with certain salinity and then filled with the gas under normal conditions.
As a specific embodiment of the method, when the step (1) is to put the sample to be tested containing the loose deposit of the hydrate into the sample holder, the confining pressure is applied to the sample by starting the confining pressure pump, and the cooling circulating pump and the constant temperature water tank are started so as to cool the sample and keep the constant temperature environment.
In the step (2), the configuration of the working parameters of the signal excitation module includes setting the waveform, amplitude, frequency value, frequency variation range and frequency interval of the signal;
the configuration of the working parameters of the multi-path switching module comprises setting the logic sequence of each programmable control switch adopted by the multi-path switching module;
The configuration of the working parameters of the data acquisition module comprises setting a channel number, a sampling frequency and a sampling amplitude range according to the actual channel connection condition.
As a specific embodiment of the above method of the present invention, in the step (3), two concentric ring disk electrodes form an electrode pair, and the measuring the electrical parameters of the whole sample at different excitation signal frequencies includes:
And the two concentric ring disk electrodes are gated by the multipath switching module and are connected with the signal excitation module and the data acquisition module, the electric parameters of the whole sample under different excitation signal frequencies are measured in a sweep frequency mode by adopting a two-electrode method, and the connection between the two concentric ring disk electrodes and the signal excitation module and the connection between the two concentric ring disk electrodes and the data acquisition module are cut off after the measurement are completed.
As a specific embodiment of the above method of the present invention, when the two concentric ring disk electrodes each include a central disk electrode and three ring electrodes, the step (3) of forming the two concentric ring disk electrodes into electrode pairs, respectively measuring the electrical parameters of the whole sample at different excitation signal frequencies includes:
And respectively connecting the central disc electrode and the three annular electrodes in the two concentric disc electrodes to form two integral electrodes, and respectively measuring the electrical parameters of the whole sample under different excitation signal frequencies by using the two integral electrodes to form an electrode pair.
In one embodiment of the present invention, when the two concentric ring disk electrodes each include a center disk electrode and three ring electrodes, the two concentric ring disk electrodes form electrode pairs in step (3), and the electrical parameters of the whole sample at different excitation signal frequencies are measured respectively, comprising the following specific steps:
gating the first electrode system and the second electrode system (namely, respectively forming a central disc electrode and three annular electrodes in two concentric disc electrodes as a whole into the first electrode system and the second electrode system by a first multipath switching module, and forming an electrode pair by the first electrode system and the second electrode system) and the signal excitation module, the first current measurement module and the second current measurement module; gating the first electrode system, the second electrode system and the voltage measuring module through the second multipath switching module; measuring the current flowing through the electrode pairs through the first current measuring module and/or the second current measuring module, and correspondingly acquiring current data measured by the first current measuring module and the second current measuring module through the first data acquisition module and the second data acquisition module respectively; and the voltage at two ends of the electrode pair is measured by a voltage measuring module, and then the voltage data measured by the voltage measuring module is collected by a second data collecting module.
In the process, the current data obtained by measuring the first current measuring module or the second current measuring module can be used as the current data flowing through the electrode pair; the current data measured by the first current measurement module and the second current measurement module can be averaged to be used as the current data flowing through the electrode pair.
As a specific embodiment of the above method of the present invention, in the step (3), the measuring the electrical parameters of the interface between the electrode and the sample to be measured at different excitation signal frequencies using two concentric ring disk electrodes, respectively, includes:
The method comprises the steps that a disc electrode and a circular electrode of a first concentric ring disc electrode are gated through a multi-channel switching module and are connected with a signal excitation module and a data acquisition module, the electrical parameters of an interface between the first concentric ring disc electrode and a sample to be measured under different excitation signal frequencies are measured in a sweep mode by adopting a two-electrode method or a four-electrode method or sequentially adopting the two-electrode method and the four-electrode method, and the connection between the first concentric ring disc electrode and the signal excitation module and the data acquisition module is cut off after the measurement is completed;
The disc electrode and the annular electrode of the second concentric ring disc electrode are gated by the multipath switching module and are connected with the signal excitation module and the data acquisition module, the electrical parameters of the interface between the second concentric ring disc electrode and the sample to be measured under different excitation signal frequencies are measured in a sweep mode by adopting a two-electrode method or a four-electrode method or sequentially adopting the two-electrode method and the four-electrode method, and the connection between the second concentric ring disc electrode and the signal excitation module and the data acquisition module is cut off after the measurement is completed.
As a specific embodiment of the above method of the present invention, when the two concentric ring disk electrodes each include a central disk electrode and three ring electrodes and the two-electrode method is used for measurement, in step (3), the electrical parameters of the interface between the two concentric ring disk electrodes and the sample to be measured at different excitation signal frequencies are measured respectively, including:
respectively taking the center disc electrode of the two concentric disc electrodes and any two electrodes in the three annular electrodes as electrode pairs to measure the electrical parameters of the interfaces between the corresponding concentric disc electrodes and the sample to be measured under different excitation signal frequencies;
When the two concentric ring disk electrodes comprise a central disk electrode and three annular electrodes and are measured by a four-electrode method, in the step (3), the two concentric ring disk electrodes are respectively used for measuring the electrical parameters of the interface between the electrodes and the sample to be measured under different excitation signal frequencies, and the method comprises the following steps:
Respectively taking two electrodes of the center disc electrodes of the two concentric disc electrodes and two electrodes of the three annular electrodes as excitation electrode pairs, and taking the other two electrodes as measurement electrode pairs to measure the electrical parameters of the interfaces between the corresponding concentric disc electrodes and the sample to be measured under different excitation signal frequencies;
wherein at least one electrode of the excitation electrode pair and the measurement electrode pair is not the same electrode.
In a specific embodiment of the present invention, when two concentric ring disk electrodes each include a central disk electrode and three annular ring electrodes and the two-electrode method is adopted for measurement, in step (3), the two concentric ring disk electrodes are adopted for measuring electrical parameters of an interface between the electrodes and a sample to be measured at different excitation signal frequencies, respectively, including the following specific steps:
A central disc electrode in a first electrode system and any two electrodes in three annular electrodes (the central disc electrode in the first electrode system and any two electrodes in the three annular electrodes form an electrode pair) are gated by a first multipath switching module, and the central disc electrode, the signal excitation module and the first current measurement module are connected with each other through a first multipath switching module; a second multipath switching module is used for gating a central disc electrode in the first electrode system, any two electrodes in the three annular electrodes and a voltage measuring module; measuring the current flowing through the electrode pair through a first current measuring module, measuring the voltage at two ends of the electrode pair through a voltage measuring module, and correspondingly acquiring current and voltage data measured by the first current measuring module and the voltage measuring module through a first data acquisition module and a second data acquisition module respectively;
Then, a central disc electrode in the second electrode system and any two electrodes in the three annular electrodes (the central disc electrode in the second electrode system and any two electrodes in the three annular electrodes form an electrode pair) are gated by the first multipath switching module, and the central disc electrode, the signal excitation module and the second current measurement module are also gated by the first multipath switching module; a second multipath switching module is used for gating a central disc electrode in a second electrode system, any two electrodes in three annular electrodes and a voltage measuring module; and measuring the current flowing through the electrode pair through a second current measuring module, measuring the voltage at two ends of the electrode pair through a voltage measuring module, and correspondingly acquiring the current and voltage data measured by the second current measuring module and the voltage measuring module through a second data acquisition module.
When two concentric ring disk electrodes comprise a central disk electrode and three annular electrodes and are measured by a four-electrode method, in the step (3), the two concentric ring disk electrodes are respectively used for measuring the electrical parameters of the interface between the electrodes and the sample to be measured under different excitation signal frequencies, and the method comprises the following specific steps:
The exciting electrode and the measuring electrode in the first electrode system (the exciting electrode and the measuring electrode in the first electrode system form an electrode pair) are gated by a first multipath switching module, a signal exciting module and a first current measuring module; the exciting electrode, the measuring electrode and the voltage measuring module in the first electrode system are gated through the second multipath switching module; measuring the current flowing through the electrode pair through a first current measuring module, measuring the voltage at two ends of the electrode pair through a voltage measuring module, and correspondingly acquiring current and voltage data measured by the first current measuring module and the voltage measuring module through a first data acquisition module and a second data acquisition module respectively;
then, the exciting electrode and the measuring electrode in the second electrode system (the exciting electrode and the measuring electrode in the second electrode system form an electrode pair), the signal exciting module and the second current measuring module are gated through the first multipath switching module; the exciting electrode, the measuring electrode and the voltage measuring module in the second electrode system are gated through the second multipath switching module; and measuring the current flowing through the electrode pair through a second current measuring module, measuring the voltage at two ends of the electrode pair through a voltage measuring module, and correspondingly acquiring the current and voltage data measured by the second current measuring module and the voltage measuring module through a second data acquisition module.
The invention can realize the measurement of the whole sample to be measured and the electrical characteristic parameters of the interface between the sample to be measured and the electrode through the electrode system and the specific working modes of the electrodes in the electrode system.
The two-electrode method and the four-electrode method used in the present invention are both conventional methods, specifically, the two-electrode method means: the excitation electrodes are used as measuring electrodes at the same time, namely, current is injected into a sample to be measured through a pair of excitation electrodes, and voltage is collected on the pair of electrodes at the same time; the four-electrode method refers to: at least one of the excitation electrode and the measurement electrode is not the same electrode, and similar to the two-electrode method, current is injected into the sample to be measured through the excitation electrode, and meanwhile, voltage is collected in the measurement electrode.
In the two-electrode method and the four-electrode method described above, a voltage may be applied to a sample to be measured by an excitation electrode, and then a current passing through the sample is measured from a measurement electrode. The voltage and the current are measured by a voltage measuring module and a current measuring module respectively, and the measured data are collected by a data collecting module (such as a data collecting card).
In the measuring process, when the signal excitation module outputs current, the current is a known quantity (set value), the current measuring module and the voltage measuring module are utilized to measure the current (actual current) and the voltage of the corresponding electrode pair, the current measuring module and the voltage measuring module are connected with the data acquisition card, and the data acquisition card acquires measurement data; when the signal excitation module outputs voltage, the voltage is a known quantity (set value), the current and voltage (actual voltage) of the corresponding electrode pair are measured by the current measuring module and the voltage measuring module, the current measuring module and the voltage measuring module are connected with the data acquisition card, and the data acquisition card acquires measurement data.
In step (5), the data acquisition module is used to acquire the current and voltage data measured in step (4), and the electrical parameters of the sample to be measured are obtained after the current and voltage data are processed, which comprises:
filtering the voltage waveform and the current waveform, and selecting proper signal length according to the characteristics of the waveform;
obtaining peak values and initial phase angles of the voltage waveform and the current waveform through a waveform peak value detection algorithm and a phase discrimination algorithm;
Dividing the voltage peak value by the current peak value by utilizing ohm law to obtain an impedance modulus value, and calculating the difference between the initial phase angles of the voltage and the current to obtain an impedance phase angle;
Determining the composition of the impedance from the impedance phase angle, comprising: if the impedance phase angle is 0, determining that the impedance is only composed of resistors, and if the impedance phase angle is negative, determining that the impedance comprises both resistors and capacitors;
Respectively calculating to obtain the impedance and the resistance of the real sample to be measured through the formula (1) and the formula (2);
z r=Zw-Zi1-Zi2 formula (1);
r r=Rw-Ri1-Ri2 formula (2);
In the formula (1), Z r is the impedance of the real sample to be measured, Z w is the measured impedance of the whole sample to be measured, and Z i1,Zi2 is the measured impedance of the interface between the electrode and the sample to be measured;
In the formula (2), R r is the resistance of the real sample to be measured, R w is the measured resistance of the whole sample to be measured, and R i1,Ri2 is the measured resistance of the interface between the electrode and the sample to be measured;
Under the condition that the impedance phase angle is 0, namely the impedance is only composed of resistors, calculating to obtain the resistor of the real sample to be measured through a formula (2); under the condition that the impedance phase angle is a negative value, namely the impedance comprises both a resistor and a capacitor, calculating according to a formula (1) to obtain the impedance of the real sample to be measured;
According to the impedance, the resistance and the geometric factors of the real sample to be measured, respectively through a formula (3) and a formula (4), calculating to obtain the complex resistivity or the resistivity of the real sample to be measured;
ρ r=Rr×F3 formula (4);
In the formula (3), ρr * is the complex resistivity of the real sample to be measured, Z r is the impedance of the real sample to be measured, and F 3 is the geometric factor of the real sample to be measured;
In the formula (4), ρr is the resistivity of the real sample to be measured, R r is the resistance of the real sample to be measured, and F 3 is the geometric factor of the real sample to be measured.
As a specific embodiment of the above method of the present invention, the filtering process includes smoothing filtering, wavelet mode maximum filtering, butterworth filtering, etc.
As a specific embodiment of the above method of the present invention, the characteristics of the waveform include whether the waveform is distorted, and the like.
As a specific embodiment of the above method of the present invention, the method further includes: and measuring pore pressure, temperature, confining pressure and cooling liquid temperature in the sample to be measured by using a pressure sensor and a temperature sensor, filtering pore pressure and temperature data, and finally calculating to obtain the hydrate saturation of the sample to be measured by using the filtered pore pressure and temperature data.
In the invention, the known porosity and the molecular composition of the hydrate are combined, and the gas consumption method is adopted, namely the amount of the generated hydrate is calculated by calculating the amount of the consumed methane gas, so that the hydrate saturation of the simulated sediment is obtained.
As a specific embodiment of the above method of the present invention, the filtering includes smoothing filtering, wavelet mode maximum filtering, butterworth filtering, etc.
In step (5), the data acquisition module is used to acquire the current and voltage data measured in step (4), and the electrical parameters of the sample to be measured are obtained after the current and voltage data are processed, which further includes:
For the measurement of the electrical parameters of the whole sample to be measured, the geometrical factor F 1 combined with the whole sample to be measured can be converted into resistivity from resistance or into complex resistivity from impedance;
For the measurement of the electrical parameters of the interface between the sample to be measured and the electrode, the geometrical factor F 2 of the combined interface region is converted from resistance to resistivity or from impedance to complex resistivity.
Description: the impedance multiplied by the geometry factor equals the complex resistivity and the resistance multiplied by the geometry factor equals the resistivity.
The meaning of F 1、F2、F3 mentioned above and the calculation method are as follows:
F 1 is the geometric factor of the whole sample to be measured, wherein the whole sample to be measured comprises an interface area and a real sample;
F 2 is the geometric factor of the interface region;
And F 3 is the geometric factor of the real sample to be measured, namely the geometric factor of the rest part of the whole sample to be measured after the interface area is removed.
The calculation formula of F 1、F2、F3 is given in detail below in conjunction with fig. 4, and is shown in formulas (2) - (4), respectively:
f 1=S/L1 formula (2);
f 2=S/L2 formula (3);
f 3=S/L3 formula (4);
Wherein: L 2 can sample one eighth of the diameter D s.
In the invention, the impedance obtained by measuring the whole sample to be measured (including the real sample to be measured and the interface between the sample to be measured and the electrode) is Z w, and the impedance obtained by measuring the interface between the electrode to be measured and the sample to be measured is Z i1 and Z i2 (corresponding to the first concentric ring plate electrode and the second concentric ring plate electrode respectively). If the impedance is composed of only resistors, the resistor obtained by measuring the whole sample to be measured is R w, and the resistor obtained by measuring the interface between the electrode and the sample to be measured is R i1 and R i2 (corresponding to the first concentric ring plate electrode and the second concentric ring plate electrode respectively). The series connection method in the equivalent circuit is adopted, namely the impedance Z w or the resistance R w of the whole sample to be tested is considered to be composed of three parts, namely Z w=Zi1+Zr+Zi2 or R w=Ri1+Rr+Ri2, wherein Z r and R r respectively represent the impedance or the resistance of the real sample to be tested except for interface influences. Thus, the real sample to be measured, such as the impedance Z r or the resistance R r of the real hydrate-containing loose deposit, can be obtained by using a serial connection method. It should be noted that, when the frequencies of the excitation signals are different, the values of the impedances Z w、Zi1、Zr、Zi2 are often different.
As a specific embodiment of the above method of the present invention, the hydrate saturation of the sample to be measured is calculated according to the following formula (1) using the pore pressure and temperature data after filtration;
In the formula (1), S h is the saturation of the hydrate of the sample to be detected; m h is the molar mass of the hydrate, unit: kg/mol; ρ h is the density of the hydrate, unit: kg/m 3;T1 is the temperature of the sample to be tested when the hydrate is not produced or has been completely decomposed, unit: k, performing K; t 2 is the temperature of the sample to be measured in the process of hydrate generation or decomposition, and the unit is: k, performing K; p 1 is pore pressure of the sample to be measured when hydrate is not generated or is completely decomposed, and the unit is: pa; p 2 is the pressure of the gas in the inner shell in the process of decomposing the hydrate, unit: pa; z g1 is the compression factor of the gas, the warm-pressing conditions are P 1 and T 1;Zg2 are the compression factors of the gas, and the warm-pressing conditions are P 2 and T 2; r is molar gas constant, unit: J/(mol.K).
Compared with the prior art, the electrical parameter detection and treatment system and method for the loose deposit of the hydrate provided by the invention have the beneficial effects that:
The electrode system provided by the invention can be used for obtaining the electrical parameters of the whole sample to be measured (including the real sample to be measured and the interface between the sample to be measured and the electrode) and also can be used for obtaining the electrical parameters of the interface between the sample to be measured and the electrode. By utilizing the electrode system and combining the designed electrode working mode, the whole sample to be tested and abundant electrical parameter data of the interface can be obtained at the same time, thereby providing a data base for subsequent data processing and eliminating the influence of the electrical property of the interface.
The invention also provides a data processing method for eliminating the influence of the electrical property of the interface, and realizes the correction of the electrical parameter and the electrical property of the sample to be tested, so that the acquired electrical parameter of the sample to be tested can truly and accurately reflect the electrical property of the sample to be tested and is not influenced by the electrical property of the interface any more.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for the description of the embodiments will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an electrical parameter detection and processing system for loose deposits of hydrates provided in an embodiment of the present invention.
Fig. 2a is a schematic structural view of a first concentric ring disk electrode used in an embodiment of the present invention.
FIG. 2b is a schematic diagram of a second concentric ring disk electrode used in an embodiment of the invention.
FIG. 3 is a schematic view of the structure of a sample holder used in an embodiment of the present invention.
FIG. 4 is a schematic diagram of the sample used in the calculation of F 1、F2、F3 according to the present invention.
The main reference numerals illustrate:
In fig. 3:
1. The first lead wire, 2 is the second lead wire, A is the first concentric ring disk electrode (first electrode system), A' is the second concentric ring disk electrode (second electrode system), C is the sample to be tested, 3 is the rubber sleeve, 4 is the inner shell, 5 is the outer shell, 6 is the confining pressure pump, 7 is the cooling circulation pump, 8 is a vacuum pump, 9 is a booster pump or a liquid injection pump, 10 is a constant temperature water tank, 11 is a gas cylinder or a liquid cylinder, 12 is a confining pressure fluid tank, ① is a confining pressure fluid conduit, ② is a cooling liquid conduit, ③ is a vacuum conduit, and ④ is a gas injection or water injection conduit.
Detailed Description
In order to make the technical features, objects and advantageous effects of the present invention more clearly understood, the technical aspects of the present invention will now be described in detail with reference to the following specific examples, but should not be construed as limiting the scope of the present invention.
It should be noted that the term "comprising" in the description of the invention and the claims and any variations thereof in the above-described figures is intended to cover a non-exclusive inclusion, such as a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements that are expressly listed or inherent to such process, method, article, or apparatus.
In the present invention, the terms "inner", "outer", "middle", "left" and "right" and the like indicate the azimuth or positional relationship based on the azimuth or positional relationship shown in the drawings. These terms are only used to better describe the present invention and its embodiments and are not intended to limit the scope of the indicated devices, elements or components to the particular orientations or to configure and operate in the particular orientations.
Furthermore, the terms "disposed," "connected," and "connected" are to be construed broadly. For example, "connected" may be in a fixed connection, a removable connection, or a unitary construction; may be a mechanical connection, or an electrical connection; may be directly connected, or indirectly connected through intervening media, or may be in internal communication between two devices, elements, or components. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
Example 1
The embodiment provides an electrical parameter detecting and processing system for loose deposit of hydrate, the structure of the system is schematically shown in fig. 1, and as can be seen from fig. 1, the system includes:
a sample holder and a parameter detection and processing device; the sample holder is used for containing a sample C to be measured of loose sediment of the hydrate, and the sample is cylindrical;
the parameter detection and processing device comprises a first electrode system, a second electrode system, a first multipath switching module, a second multipath switching module, a signal excitation module, a first data acquisition module, a second data acquisition module, a first current measurement module, a second current measurement module, a voltage measurement module and a controller;
The first electrode system and the second electrode system are respectively arranged at two end surfaces of a cylindrical sample in a contact manner, the first electrode system and the second electrode system are concentric ring disk electrodes which are respectively marked as a first concentric ring disk electrode A and a second concentric ring disk electrode A ', the first concentric ring disk electrode A and the second concentric ring disk electrode A' comprise a central disk electrode and three ring-shaped electrodes with gradually increased sizes (the sizes refer to the diameters of the ring-shaped electrodes and not the widths of the ring-shaped electrodes), and the three ring-shaped electrodes with gradually increased sizes are sequentially sleeved outside the disk electrode and the ring-shaped electrode according to the sequence from small sizes to large sizes; the gaps between the central disc electrode and the annular electrode and between the annular electrode and the annular electrode are provided with electric insulation materials;
for convenience of description, the first concentric ring disk electrode a and the second concentric ring disk electrode a' are shown in fig. 2a and fig. 2b, respectively, and as can be seen from fig. 2a and fig. 2b, the first concentric ring disk electrode and the second concentric ring disk electrode each include a central disk electrode and three circular ring electrodes, wherein A4 is the central disk electrode, and A1, A2 and A3 are the circular ring electrodes, respectively; in the second concentric ring disk electrode, A '4 is a central disk electrode, and A'1, A '2 and A'3 are respectively annular electrodes; the electrodes A1, A2, A3, A4, A '1, A'2, A '3 and A'4 are all sheet metal electrodes, the electrodes A1, A2, A3 and A4 are positioned on the same plane and are contacted with one end face (left end face) of the cylindrical sample to be detected, and the electrodes A '1, A'2, A '3 and A'4 are positioned on the same plane and are contacted with the other end face (right end face) of the cylindrical sample to be detected;
The diameters of the center disc electrodes A4 and A '4 are 10mm, the widths of the annular electrodes A3 and A'3 are 5mm, the widths of the annular electrodes A2 and A '2 are 5mm, and the widths of the annular electrodes A1 and A'1 are 15mm;
The width of the insulating layer (electric insulating material layer, which is made of PEEK material or polytetrafluoroethylene material) between the electrodes is 2.5mm;
In this embodiment, the schematic structure of the sample holder is shown in fig. 3, and as can be seen from fig. 3, the sample holder includes a holder body and two ends detachably connected to two ends of the holder body respectively; the two ends are respectively provided with a lead guide pipe for leading leads connected with the electrodes out of the sample holder;
The clamp holder body comprises a rubber sleeve 3, an inner shell 4 and an outer shell 5, wherein the inner shell 4 and the outer shell 5 are cylindrical, and the outer shell 5 is sleeved outside the inner shell 4 and forms a first gap between the outer shell 5 and the inner shell 4;
The rubber sleeve 3 is used for fixing a hydrate-containing loose sediment sample C to be tested, the rubber sleeve 3 is positioned in the inner shell 4, and a second gap is reserved between the rubber sleeve 3 and the inner shell 4;
The inner housing 4 and the outer housing 5 are respectively provided with a confining pressure fluid opening and a cooling liquid opening, and the confining pressure fluid opening and the cooling liquid opening are respectively connected with the confining pressure fluid tank 12 and the constant temperature water tank 10 through the confining pressure fluid conduit ① and the cooling liquid conduit ② by the confining pressure pump 6 and the cooling circulating pump 7 so as to respectively introduce confining pressure fluid and cooling liquid into the second gap and the first gap;
The inner shell 4, the outer shell 5 and the rubber sleeve 3 are correspondingly provided with a vacuumizing port and an injection port, and the vacuumizing port is connected with a vacuum pump 8 through a vacuum conduit ③; the injection port is connected with a gas bottle or a liquid bottle 11 through a gas injection or water injection conduit ④ and a booster pump or a liquid injection pump 9;
The sample holder is also provided with a plurality of pressure sensors and a plurality of temperature sensors for measuring the temperature, the confining pressure and the temperature of the cooling liquid in the sample to be measured; the temperature sensor adopts a thermal resistor or a thermocouple, and the accuracy is +/-1 ℃;
in this embodiment, the rubber sleeve is made of buna rubber or fluororubber;
In this embodiment, the inner shell, the outer shell and the end are made of stainless steel, and the stainless steel includes 304 type, 316 type or 316L type stainless steel;
in this embodiment, the width of the first gap is 2cm;
In this embodiment, the controller is electrically connected to the first multi-path switching module via a signal excitation module, the first multi-path switching module is electrically connected to the first electrode system and the second electrode system via a first current measurement module and a second current measurement module (such as the first lead 1 and the second lead 2 in fig. 3, which are certainly not limited to the two leads), the first electrode system and the second electrode system are also electrically connected to the controller via a second multi-path switching module, a voltage measurement module and a second data acquisition module, the first current measurement module and the second current measurement module are electrically connected to the controller via a first data acquisition module and a second data acquisition module, respectively, and the first multi-path switching module and the second multi-path switching module are electrically connected to the controller;
In this embodiment, the first multi-path switching module is electrically connected to the two concentric ring disk electrode units (i.e., the first electrode unit and the second electrode unit) through the first current measuring module and the second current measuring module respectively, and the two concentric ring disk electrode units are electrically connected to the controller through the second multi-path switching module, the voltage measuring module and the second data acquisition module;
In addition, the first multi-path switching module can be electrically connected with the disc electrode and the annular electrode in the two concentric ring disc electrodes (namely the first electrode system and the second electrode system) through the first current measuring module and the second current measuring module respectively through leads, and the disc electrode and the annular electrode in the two concentric ring disc electrodes are electrically connected with the controller through the second multi-path switching module, the voltage measuring module and the second data acquisition module;
In this embodiment, the multi-path switching module (i.e., the first multi-path switching module and the second multi-path switching module) adopts a programmable control multi-path switch, the switch is connected with each electrode, and the closing and opening states of each switch can be conveniently controlled through a software program, so that gating and blocking of each electrode are realized;
In this embodiment, the data acquisition module (i.e., the first data acquisition module and the second data acquisition module) may be a data acquisition card, and has the characteristics of multiple channels and high sampling rate (to meet the requirement of the frequency of the excitation signal, for example, the highest frequency of the excitation signal is 10MHz, the highest sampling frequency of the data acquisition card should not be lower than 50MHz, i.e., the highest frequency of the data acquisition card should be 5 times or more than the highest frequency of the excitation signal), and the working parameters of the data acquisition card may be configured by a software program, for example, the synchronous sampling, the sampling rate is 50MHz, the sampling point number is 50k, the input amplitude range is-5V to 5V, etc.;
In this embodiment, the signal excitation module adopts a programmable signal generator, and can select output voltage or output current, and the output signal has the characteristics of adjustable amplitude, adjustable waveform, adjustable frequency point and frequency range, and the like;
in this embodiment, the controller is a computer equipped with measurement and control software, and may be an industrial control computer with stable performance and continuous operation, where the measurement and control software is developed by using vc++ and LabVIEW platforms, and parameter configuration and working mode setting are performed on the multi-path switching module, the data acquisition card, the signal excitation module, and the like by using the measurement and control software.
Example 2
The embodiment provides a method for detecting and processing electrical parameters of loose deposit of hydrate, wherein the method is realized by using the system for detecting and processing electrical parameters of loose deposit of hydrate provided in embodiment 1, and the method comprises the following specific steps:
(1) Preparing a sample to be tested containing loose hydrate sediment:
1) Opening the sample holder, and adding natural sea sand into a rubber sleeve of the sample holder to simulate loose sediment;
2) After all parts of a sample holder are assembled, firstly vacuumizing the raw material components by using a vacuum pump, then starting a liquid injection pump and a booster pump to inject NaCl aqueous solution with the mass fraction of 3.5% and methane into the natural sea sand, so that the natural sea sand pores are filled with the NaCl aqueous solution with the mass fraction of 3.5%, methane gas is dissolved in the aqueous solution, then starting a confining pressure pump to apply confining pressure to the sample, adopting inert silicone oil as a medium for generating confining pressure, starting a cooling circulation pump and a constant-temperature water tank to circulate cooling liquid in a jacket (a first gap), and further cooling the sample and keeping a constant-temperature environment, wherein the cooling liquid adopts water containing ethylene glycol in the embodiment;
In the embodiment, typical working conditions are that the confining pressure is 10MPa, the pore pressure in the simulated sediment is 8MPa, and the temperature of the cooling liquid is 1 ℃;
The cylindrical sample to be measured prepared in this example has a length of 120mm and a diameter of 60mm. The rubber sleeve in the sample holder tightly wraps the sample to be tested, and plays a role in sealing the sample to be tested in the rubber sleeve under the confining pressure.
(2) Working parameters of the signal excitation module, the multipath switching module and the data acquisition module are configured:
The working parameters of the configuration signal excitation module comprise waveform, amplitude, frequency value, frequency variation range and frequency interval of the set signal; in this embodiment, the signal excitation module outputs a current, the waveform is a sine wave, the amplitude is 1V, the frequency range is 0.001Hz to 10MHz, 1 test frequency point per 10 octaves, i.e. 0.001Hz, 0.01Hz, 0.1Hz, etc., until 1MHz, 10MHz;
the configuration of the operating parameters of the multiple switching modules (i.e., the first multiple switching module and the second multiple switching module) includes setting the logic sequence of each programmable switch used to switch them;
The configuration of the working parameters of the data acquisition modules (namely the first data acquisition module and the second data acquisition module) comprises setting a channel number, a sampling frequency and a sampling amplitude range according to the connection condition of an actual channel; in the embodiment, the working parameters of the data acquisition module (data acquisition card) can be configured through a software program, the synchronous sampling is performed, the sampling rate is 50MHz, the sampling point number is 50k, and the input amplitude range is-5V to 5V;
(3) Two concentric ring disk electrodes form electrode pairs, and the electrical parameters of the whole sample under different excitation signal frequencies are respectively measured; and respectively adopting two concentric ring disk electrodes to measure the electrical parameters of the interface between the electrode and the sample to be measured under different excitation signal frequencies:
When the electrical parameters of the whole sample under different excitation signal frequencies are measured, the electrodes A1, A2, A3 and A4 in the first concentric ring disk electrode are connected to form 1 electrode, which is marked as E I, and the electrodes A '1, A'2, A '3 and A'4 in the second concentric ring disk electrode are connected to form 1 electrode, which is marked as E II, and then the two electrodes E I and E II form an electrode pair, so that the whole sample to be measured is measured;
When the two-electrode method is adopted to measure the electrical parameters of the interface between the electrode and the sample to be measured under different excitation signal frequencies, A4 and A1 can be used as electrode pairs, A4 and A2 can be used as electrode pairs, A4 and A3 can be used as electrode pairs, A3 and A2 can be used as electrode pairs, A3 and A1 can be used as electrode pairs, and A2 and A1 can be used as electrode pairs for the first concentric ring disk electrode;
When the four-electrode method is adopted to measure the electrical parameters of the interface between the electrode and the sample to be measured under different excitation signal frequencies, A4 and A1 can be used as an excitation electrode pair, A3 and A2 can be used as a measurement electrode pair at the same time, A4 and A1 can be used as an excitation electrode pair, A4 and A2 can be used as a measurement electrode pair at the same time, A4 and A1 can be used as an excitation electrode pair, and A3 and A1 can be used as a measurement electrode pair at the same time for the first concentric ring disk electrode.
The processing method is consistent with the first concentric ring disk electrode for the second concentric ring disk electrode.
In specific implementation, the embodiment adopts a two-electrode method to measure the electrical parameters, firstly, electrodes A4 and A1 in a first concentric ring disk electrode are used as electrode pairs, and then electrodes A '4 and A'1 of a second concentric ring disk electrode are used as electrode pairs to respectively measure the electrical parameters of two interfaces between the electrodes and a sample to be measured.
(4) Measuring, by a voltage measuring module, a voltage across the sample to be measured from the respective measuring electrode:
(5) And (3) acquiring the voltage data obtained in the step (4) by utilizing a data acquisition module, and processing the voltage data to obtain the electrical parameters of the sample to be detected:
And filtering the voltage waveform and the current waveform by using a ten-point moving average filtering method, and selecting the signal length of 3 periods. If the test frequency is 1Hz, selecting the signal length to be 3s;
respectively obtaining peak values and initial phase angles of a voltage waveform and a current waveform by utilizing an FFT spectrum analysis method in a waveform peak detection algorithm and a phase discrimination algorithm;
Dividing the voltage peak value by the current peak value by utilizing ohm law to obtain an impedance modulus value, and calculating the difference between the initial phase angles of the voltage and the current to obtain an impedance phase angle;
the impedance composition is determined based on the impedance phase angle, and if the impedance phase angle is 0, it is known that the impedance is composed of only resistors, and if the impedance phase angle is negative, the impedance includes both resistors and capacitors.
The following description will explain a specific embodiment in which the impedance phase angle is 0. It should be noted that the impedance and resistance values measured at different test frequencies are different, which is due to the electric polarization effect inside the sample and at the interface between the sample and the electrode. The following embodiments are described with respect to only one fixed frequency, i.e., without considering the frequency effects, and similar data processing methods can be used under other frequency conditions.
Under the condition that the impedance phase angle is 0, namely the impedance is only composed of resistors, calculating to obtain the resistor of the real sample to be measured through a formula (2);
r r=Rw-Ri1-Ri2 formula (2);
In the formula (2), R r is the resistance of the real sample to be measured, R w is the measured resistance of the whole sample to be measured, and R i1,Ri2 is the measured resistance of the interface between the electrode and the sample to be measured;
according to the resistance of the real sample to be measured and the geometric factor of the real sample to be measured, calculating to obtain the resistivity of the real sample to be measured through the formula (4);
ρ r=Rr×F3 formula (4);
in the formula (4), ρr is the resistivity of the real sample to be measured, R r is the resistance of the real sample to be measured, and F 3 is the geometric factor of the real sample to be measured;
Wherein, the geometric factor F 3 = S/L of the real sample to be measured, S is the cross-sectional area of the sample to be measured (diameter is 0.06 m), L is the length of the real sample to be measured (length is 0.12 m).
(6) Measuring pore pressure, temperature, confining pressure and cooling liquid temperature in a sample to be measured by using a pressure sensor and a temperature sensor, smoothing and filtering pore pressure and temperature data by using a five-point moving average filtering method, and finally calculating to obtain the hydrate saturation of the sample to be measured according to the following formula (1) by using the filtered pore pressure and temperature data; in this example, assume that the molecular formula of methane hydrate is CH 4·nH2 O, and the hydration index n takes on a value of 6;
In the formula (1), S h is the saturation of the hydrate of the sample to be detected; m h is the molar mass of the hydrate, unit: kg/mol; ρ h is the density of the hydrate, unit: kg/m 3;T1 is the temperature of the sample to be tested when the hydrate is not produced or has been completely decomposed, unit: k, performing K; t 2 is the temperature of the sample to be measured in the process of hydrate generation or decomposition, and the unit is: k, performing K; p 1 is pore pressure of the sample to be measured when hydrate is not generated or is completely decomposed, and the unit is: pa; p 2 is the pressure of the gas in the inner shell in the process of decomposing the hydrate, unit: pa; z g1 is the compression factor of the gas, the warm-pressing conditions are P 1 and T 1;Zg2 are the compression factors of the gas, and the warm-pressing conditions are P 2 and T 2; r is molar gas constant, unit: J/(mol.K).
The foregoing description of the embodiments of the invention is not intended to limit the scope of the invention, so that the substitution of equivalent elements or equivalent variations and modifications within the scope of the invention shall fall within the scope of the patent. In addition, the technical features and the technical features, the technical features and the technical invention can be freely combined for use.

Claims (17)

1. An electrical parameter detection and processing system for loose deposits of hydrates, the system comprising a sample holder and a parameter detection and processing device; the sample holder is used for containing a sample to be measured of the loose deposit of the hydrate, and the sample is cylindrical; the parameter detection and processing device comprises a first electrode system, a second electrode system, a first multipath switching module, a second multipath switching module, a signal excitation module, a first data acquisition module, a second data acquisition module, a first current measurement module, a second current measurement module, a voltage measurement module and a controller;
The first electrode system and the second electrode system are respectively arranged at two end surfaces of the cylindrical sample in a contact manner, the first electrode system and the second electrode system are concentric ring disk electrodes, the concentric ring disk electrodes comprise a central disk electrode and at least one ring electrode, and the ring electrodes are sleeved outside the disk electrode and the ring electrode in the sequence from small to large in size; the gaps between the disc electrode and the annular electrode and between the annular electrode and the annular electrode are provided with electric insulation materials;
The controller is electrically connected with the first multi-path switching module through the signal excitation module, the first multi-path switching module is electrically connected with the first electrode system and the second electrode system through the first current measurement module and the second current measurement module through leads respectively, the first electrode system and the second electrode system are also electrically connected with the controller through the second multi-path switching module, the voltage measurement module and the second data acquisition module, the first current measurement module and the second current measurement module are electrically connected with the controller through the first data acquisition module and the second data acquisition module respectively, and the first multi-path switching module and the second multi-path switching module are electrically connected with the controller respectively;
the sample holder comprises a holder body and ends which are detachably connected with two ends of the holder body respectively; the end head is provided with a lead wire guide pipe for leading a lead wire connected with the electrode out of the sample holder;
the clamp holder body comprises a rubber sleeve, an inner shell and an outer shell, wherein the inner shell and the outer shell are cylindrical, and the outer shell is sleeved outside the inner shell and forms a first gap between the outer shell and the inner shell;
The rubber sleeve is used for fixing a sample to be tested containing hydrate loose sediment, the rubber sleeve is positioned in the inner shell, and a second gap is reserved between the rubber sleeve and the inner shell;
The inner shell and the outer shell are respectively provided with a confining pressure fluid opening and a cooling liquid opening, and the confining pressure fluid opening and the cooling liquid opening are respectively connected with the confining pressure fluid tank and the constant temperature water tank through a confining pressure fluid conduit and a cooling liquid conduit by a confining pressure pump and a cooling circulating pump so as to respectively introduce confining pressure fluid and cooling liquid into the second gap and the first gap;
The inner shell, the outer shell and the rubber sleeve are correspondingly provided with a vacuumizing port and an injection port, and the vacuumizing port is connected with a vacuum pump through a vacuum conduit; the injection port is connected with a gas bottle or a liquid bottle through a booster pump or a liquid injection pump by a gas injection or water injection conduit;
the sample holder is also provided with a plurality of pressure sensors and a plurality of temperature sensors for measuring the temperature, the confining pressure and the temperature of the cooling liquid in the sample to be measured.
2. The system of claim 1, wherein the number of circular ring electrodes is 1-3.
3. The system according to claim 1 or 2, wherein the rubber sleeve is made of buna rubber or fluororubber.
4. The system of claim 1 or 2, wherein the inner housing, outer housing and tip are made of stainless steel, and the stainless steel comprises type 304, type 316 or type 316L stainless steel.
5. The system of claim 1 or 2, wherein the first void has a width of 2cm.
6. A method for the detection and treatment of electrical parameters of a loose deposit of an hydrate, characterized in that it is carried out with the system for the detection and treatment of electrical parameters of a loose deposit of an hydrate according to any one of claims 1 to 5, comprising:
(1) Placing a sample to be tested of the hydrate-containing loose deposit into a sample holder, or placing raw material components for preparing the sample to be tested of the hydrate-containing loose deposit into the sample holder and preparing the sample to be tested;
(2) According to the required detection conditions, working parameters of a signal excitation module, a multi-path switching module and a data acquisition module are configured;
(3) Two concentric ring disk electrodes form electrode pairs, and the electrical parameters of the whole sample under different excitation signal frequencies are respectively measured; respectively adopting two concentric ring disk electrodes to measure the electrical parameters of the interface between the electrode and the sample to be measured under different excitation signal frequencies;
(4) Measuring the current and the voltage passing through the sample to be measured from the corresponding measuring electrode by a current measuring module and a voltage measuring module;
(5) And (3) collecting the current and voltage data obtained in the step (4) by using a data collection module, and then processing the current and voltage data to obtain the electrical parameters of the sample to be tested.
7. The method of claim 6, wherein in step (1), preparing the sample to be tested for the loose deposit of the hydrate comprises the specific steps of:
1) Opening a sample holder, and adding raw material components for preparing a sample to be tested of the loose deposit of the hydrate into a rubber sleeve of the sample holder; the raw material components comprise natural sea sand and/or quartz sand;
2) After all parts of the sample holder are assembled, the raw material components are vacuumized by utilizing a vacuum pump, then a booster pump and a liquid injection pump are started to charge water solution and gas with certain salinity into the raw material components, then a confining pressure pump is started to apply confining pressure to the sample, and a cooling circulating pump and a constant-temperature water tank are started to cool the sample and keep a constant-temperature environment.
8. The method of claim 7, wherein the feedstock component further comprises kaolin.
9. The method according to claim 7 or 8, wherein the gas is methane and the aqueous solution having a certain salinity is an aqueous NaCl solution with a mass fraction of 3.5%.
10. The method of claim 6, wherein in step (2), configuring the operating parameters of the signal excitation module includes setting the waveform, amplitude, frequency value, frequency range of variation, and frequency interval of the signal;
the configuration of the working parameters of the multi-path switching module comprises setting the logic sequence of each programmable control switch adopted by the multi-path switching module;
The configuration of the working parameters of the data acquisition module comprises setting a channel number, a sampling frequency and a sampling amplitude range according to the actual channel connection condition.
11. The method of claim 6, wherein in step (3) the two concentric ring disk electrodes form electrode pairs, each measuring an electrical parameter of the entire sample at a different excitation signal frequency, comprising:
And the two concentric ring disk electrodes are gated by the multipath switching module and are connected with the signal excitation module and the data acquisition module, the electric parameters of the whole sample under different excitation signal frequencies are measured in a sweep frequency mode by adopting a two-electrode method, and the connection between the two concentric ring disk electrodes and the signal excitation module and the connection between the two concentric ring disk electrodes and the data acquisition module are cut off after the measurement are completed.
12. The method of claim 11, wherein when the two concentric ring disk electrodes each comprise a central disk electrode and three annular ring electrodes, forming the two concentric ring disk electrodes into electrode pairs in step (3) respectively measures electrical parameters of the entire sample at different excitation signal frequencies, comprising:
And respectively connecting the central disc electrode and the three annular electrodes in the two concentric disc electrodes to form two integral electrodes, and respectively measuring the electrical parameters of the whole sample under different excitation signal frequencies by using the two integral electrodes to form an electrode pair.
13. The method of claim 6, wherein in step (3), the two concentric ring disk electrodes are used to measure the electrical parameters of the interface between the electrode and the sample under test at different excitation signal frequencies, respectively, comprising:
The method comprises the steps that a disc electrode and a circular electrode of a first concentric ring disc electrode are gated through a multi-channel switching module and are connected with a signal excitation module and a data acquisition module, the electrical parameters of an interface between the first concentric ring disc electrode and a sample to be measured under different excitation signal frequencies are measured in a sweep mode by adopting a two-electrode method or a four-electrode method or sequentially adopting the two-electrode method and the four-electrode method, and the connection between the first concentric ring disc electrode and the signal excitation module and the data acquisition module is cut off after the measurement is completed;
The disc electrode and the annular electrode of the second concentric ring disc electrode are gated by the multipath switching module and are connected with the signal excitation module and the data acquisition module, the electrical parameters of the interface between the second concentric ring disc electrode and the sample to be measured under different excitation signal frequencies are measured in a sweep mode by adopting a two-electrode method or a four-electrode method or sequentially adopting the two-electrode method and the four-electrode method, and the connection between the second concentric ring disc electrode and the signal excitation module and the data acquisition module is cut off after the measurement is completed.
14. The method of claim 13, wherein when the two concentric ring disk electrodes each comprise a central disk electrode and three annular ring electrodes and the measurement is performed by a two-electrode method, in step (3), the measuring the electrical parameters of the interface between the electrodes and the sample to be measured at different excitation signal frequencies using the two concentric ring disk electrodes, respectively, comprises:
respectively taking the center disc electrode of the two concentric disc electrodes and any two electrodes in the three annular electrodes as electrode pairs to measure the electrical parameters of the interfaces between the corresponding concentric disc electrodes and the sample to be measured under different excitation signal frequencies;
When the two concentric ring disk electrodes comprise a central disk electrode and three annular electrodes and are measured by a four-electrode method, in the step (3), the two concentric ring disk electrodes are respectively used for measuring the electrical parameters of the interface between the electrodes and the sample to be measured under different excitation signal frequencies, and the method comprises the following steps:
Respectively taking two electrodes of the center disc electrodes of the two concentric disc electrodes and two electrodes of the three annular electrodes as excitation electrode pairs, and taking the other two electrodes as measurement electrode pairs to measure the electrical parameters of the interfaces between the corresponding concentric disc electrodes and the sample to be measured under different excitation signal frequencies;
wherein at least one electrode of the excitation electrode pair and the measurement electrode pair is not the same electrode.
15. The method of claim 6, wherein in step (5), the data acquisition module is used to acquire the current and voltage data measured in step (4), and the electrical parameters of the sample to be measured are obtained after the current and voltage data are processed, which comprises:
filtering the voltage waveform and the current waveform, and selecting proper signal length according to the characteristics of the waveform;
obtaining peak values and initial phase angles of the voltage waveform and the current waveform through a waveform peak value detection algorithm and a phase discrimination algorithm;
Dividing the voltage peak value by the current peak value by utilizing ohm law to obtain an impedance modulus value, and calculating the difference between the initial phase angles of the voltage and the current to obtain an impedance phase angle;
Determining the composition of the impedance from the impedance phase angle, comprising: if the impedance phase angle is 0, determining that the impedance is only composed of resistors, and if the impedance phase angle is negative, determining that the impedance comprises both resistors and capacitors;
Respectively calculating to obtain the impedance and the resistance of the real sample to be measured through the formula (1) and the formula (2);
Z r= Zw-Zi1- Zi2 formula (1);
r r= Rw-Ri1- Ri2 formula (2);
In the formula (1), Z r is the impedance of the real sample to be measured, Z w is the measured impedance of the whole sample to be measured, and Z i1,Zi2 is the measured impedance of the interface between the electrode and the sample to be measured;
in the formula (2), R r is the resistance of the real sample to be measured, R w is the measured resistance of the whole sample to be measured, and R i1,Ri2 is the measured resistance of the interface between the electrode and the sample to be measured;
According to the impedance, the resistance and the geometric factors of the real sample to be measured, respectively through a formula (3) and a formula (4), calculating to obtain the complex resistivity or the resistivity of the real sample to be measured;
formula (3);
formula (4);
in the formula (3), ρr * is the complex resistivity of the real sample to be measured, Z r is the impedance of the real sample to be measured, and F 3 is the geometric factor of the real sample to be measured;
In the formula (4), ρr is the resistivity of the real sample to be measured, R r is the resistance of the real sample to be measured, and F 3 is the geometric factor of the real sample to be measured.
16. The method of claim 6, wherein the method further comprises: and measuring pore pressure, temperature, confining pressure and cooling liquid temperature in the sample to be measured by using a pressure sensor and a temperature sensor, filtering pore pressure and temperature data, and finally calculating to obtain the hydrate saturation of the sample to be measured by using the filtered pore pressure and temperature data.
17. The method of claim 16, wherein the hydrate saturation of the sample to be measured is calculated according to the following formula (1) using the filtered pore pressure and temperature data;
formula (1);
In the formula (1), The saturation of the hydrate of the sample to be detected; /(I)The unit is the molar mass of the hydrate: kg/mol; Density of hydrate, unit: kg/m 3;T1 is the temperature of the sample to be tested when the hydrate is not produced or has been completely decomposed, unit: k, performing K; t 2 is the temperature of the sample to be measured in the process of hydrate generation or decomposition, and the unit is: k, performing K; p 1 is pore pressure of the sample to be measured when hydrate is not generated or is completely decomposed, and the unit is: pa; p 2 is the pressure of the gas in the inner shell in the process of decomposing the hydrate, unit: pa; z g1 is the compression factor of the gas, the warm-pressing conditions are P 1 and T 1;Zg2 are the compression factors of the gas, and the warm-pressing conditions are P 2 and T 2; r is molar gas constant, unit: J/(mol.K).
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Citations (3)

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Publication number Priority date Publication date Assignee Title
DE19713267A1 (en) * 1997-01-28 1998-07-30 Abb Research Ltd Method for determining the dielectric constant and / or the conductivity of at least one medium and device for carrying out the method
CN102879899A (en) * 2011-07-15 2013-01-16 三星电子株式会社 Aperture adjusting method and device
CN111238967A (en) * 2020-03-19 2020-06-05 中国石油大学(华东) Hydrate-containing sediment mechanical property detection and data processing method

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Publication number Priority date Publication date Assignee Title
US9897529B2 (en) * 2015-09-23 2018-02-20 China University Of Petroleum (East China) Test system and test method for a simulation experiment of gas hydrate in a porous medium

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19713267A1 (en) * 1997-01-28 1998-07-30 Abb Research Ltd Method for determining the dielectric constant and / or the conductivity of at least one medium and device for carrying out the method
CN102879899A (en) * 2011-07-15 2013-01-16 三星电子株式会社 Aperture adjusting method and device
CN111238967A (en) * 2020-03-19 2020-06-05 中国石油大学(华东) Hydrate-containing sediment mechanical property detection and data processing method

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