CN111380892A - System and method for measuring decomposition rate of combustible ice - Google Patents

System and method for measuring decomposition rate of combustible ice Download PDF

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Publication number
CN111380892A
CN111380892A CN201811636313.0A CN201811636313A CN111380892A CN 111380892 A CN111380892 A CN 111380892A CN 201811636313 A CN201811636313 A CN 201811636313A CN 111380892 A CN111380892 A CN 111380892A
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CN
China
Prior art keywords
sample
combustible ice
pressure
port
decomposition rate
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Application number
CN201811636313.0A
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Chinese (zh)
Inventor
王琳琳
程久辉
刘化冰
杨纯
刘智强
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中国石油大学(北京)
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Priority to CN201811636313.0A priority Critical patent/CN111380892A/en
Publication of CN111380892A publication Critical patent/CN111380892A/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/08Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
    • G01N24/082Measurement of solid, liquid or gas content

Abstract

The application discloses a system and a method for measuring the decomposition rate of combustible ice, wherein the device consists of a sample holder and a constant pressure device, the constant pressure device comprises a pump, a pressure gauge, a liquid collecting device, a first back pressure valve and an overflow liquid tank, the sample holder comprises a shell, a cooling liquid flowing cavity is arranged in the shell, a closed sample cavity is arranged in the cooling liquid flowing cavity, a hollow pipe is sleeved on the surface of the sample cavity, and a radio frequency coil is wound on the hollow pipe; a pump controls fluid flow from an overflow fluid tank to a first port of the sample holder, out a second port of the sample holder after passing through the hollow tube in the sample holder, through the first back pressure valve, and into the liquid collection device. Controlling the combustible ice sample not to generate phase change by using a constant-pressure device; measuring a magnetic resonance signal of the combustible ice sample; and determining the decomposition rate of the combustible ice sample according to the magnetic resonance signal of the combustible ice sample. Thereby more efficiently observing the decomposition rate of the combustible ice.

Description

System and method for measuring decomposition rate of combustible ice

Technical Field

The application relates to the technical field of nuclear magnetic resonance measurement, in particular to a system and a method for measuring the decomposition rate of combustible ice.

Background

This section is intended to provide a background or context to the embodiments of the application that are recited in the claims. The description herein is not admitted to be prior art by inclusion in this section.

Combustible ice is increasingly receiving attention as one of the important strategic energy sources of countries in the world. Generally, reservoirs enriched with combustible ice are present in the ocean or polar regions. The importance of energy as a core resource and economic life line for world competition is self-evident. How to advance the process of solving the technical problem of combustible ice exploitation is the challenge of energy source life pulse in China and even countries in the world at present. Therefore, the research on combustible ice is an extremely important breakthrough point in the world energy field. One of the most important problems in the exploitation of combustible ice is the problem of phase change decomposition of combustible ice. The formation environment of the combustible ice is high pressure and low temperature. In reality, the phase change rate of the combustible ice sample taken out from the stratum at normal temperature and normal pressure is far slower than that of other substances. The main ways of exploiting combustible ice include depressurization, heating, and addition of chemical and biological agents, and the main purposes of the methods are to promote decomposition of the combustible ice. Therefore, it is very important to study the decomposition rate of combustible ice.

The methods for observing the synthesis and decomposition of combustible ice are many, including electrical, optical, acoustic, etc. Electrical observation of combustible ice is generally used for detection of formation layers, and whether combustible ice exists is calculated by observing the distribution of the formation electric field to obtain a resistivity value. The formation and decomposition of combustible ice can also be studied by using the change of resistivity, but the size of combustible ice samples is small in a laboratory, and accurate data is difficult to obtain due to environmental influences. Optics is also one of the important methods for studying the synthesis and decomposition of combustible ice. When the combustible ice is slowly formed, the light transmittance is reduced; when the combustible ice is decomposed after being heated, the luminous flux rate is increased. However, combustible ice is generally present in sediments, so that some combustible ice samples have no light transmittance and cannot be measured by an optical method. Acoustic parameters such as sound velocity and amplitude can be measured by an ultrasonic method to obtain corresponding related parameters of the combustible ice.

How to efficiently observe and research the decomposition rate of combustible ice is an urgent problem to be solved.

Disclosure of Invention

The embodiment of the application provides a system and a method for measuring the decomposition rate of combustible ice, which can efficiently observe the decomposition rate of the combustible ice.

In a first aspect, the present application provides a system for measuring the rate of combustible ice decomposition comprising a sample holder and a constant pressure device comprising a pump, a pressure gauge, a liquid collection device, a first return valve, and an overflow liquid tank; the sample holder comprises a shell, a cooling liquid flowing cavity is arranged in the shell, a closed sample cavity is arranged in the cooling liquid flowing cavity, a hollow pipe is sleeved on the surface of the sample cavity, and a radio frequency coil is wound on the hollow pipe;

the pump control fluid flows from an overflow fluid tank to a first port of the sample holder, out a second port of the sample holder after passing through the hollow tube in the sample holder, through the first back pressure valve, and into the liquid collection device.

In a second aspect, the present application provides a method of measuring a combustible ice rate based on the system of measuring a combustible ice decomposition rate according to the first aspect, comprising:

putting the combustible ice sample into a sample cavity of a sample holder, and controlling the combustible ice sample not to generate phase change by using a constant-pressure device;

measuring a magnetic resonance signal of the combustible ice sample;

and determining the decomposition rate of the combustible ice sample according to the magnetic resonance signal of the combustible ice sample.

Thus in the present embodiment, by means of the sample holder and the constant pressure device comprising a pump, a pressure gauge, a liquid collection device, a first return valve and an overflow liquid tank; the sample holder comprises a shell, a cooling liquid flowing cavity is arranged in the shell, a closed sample cavity is arranged in the cooling liquid flowing cavity, a hollow pipe is sleeved on the surface of the sample cavity, and a radio frequency coil is wound on the hollow pipe; the pump control fluid flows out from the overflow liquid tank to the first end of the cooling liquid flowing cavity, flows out from the second end of the cooling liquid flowing cavity after passing through the hollow pipe in the cooling liquid flowing cavity, and flows into the liquid collecting device through the first back pressure valve. Based on the system, the constant-pressure device is used for controlling the combustible ice sample not to generate phase change, then the nuclear magnetic resonance analyzer is used for measuring the transverse magnetization vector of the combustible ice sample, and the constant-pressure device is controlled until the transverse magnetization vector of the combustible ice sample does not change any more; so as to determine the decomposition rate of the combustible ice sample according to the change of the transverse magnetization vector of the combustible ice sample along with time. Thereby more efficiently observing the decomposition rate of the combustible ice.

Drawings

In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts. In the drawings:

FIG. 1 is a schematic diagram of a system for measuring the decomposition rate of combustible ice provided in an embodiment of the present application;

FIG. 2 is a schematic diagram of a sample holder provided in an embodiment of the present application;

FIG. 3 is a graph of combustible ice pressure versus time provided in an embodiment of the present application;

fig. 4 is a graph showing the change of magnetization vector with time under the constant voltage condition provided in the example of the present application.

Detailed Description

To make the objects, technical solutions and advantages of the embodiments of the present application more apparent, the embodiments of the present application are further described in detail below with reference to the accompanying drawings. The exemplary embodiments and descriptions of the present application are provided herein to explain the present application and not to limit the present application.

Combustible ice is a substance formed by combining alkanes or hydrocarbons with water at a certain temperature and pressure. Thus, combustible ice is rich in hydrogen atoms. While hydrogen nuclei are an important condition for nuclear magnetic resonance observation. The depressurization method is the earliest method for exploiting combustible ice, and has the historical status and the physical significance of being not worn out on the exploitation research of the combustible ice. However, how to control the pressure to be stable and obtain the decomposition rate of the combustible ice in a sufficiently short time is the most urgent problem to be solved at present.

In recent years, nuclear magnetic resonance is mature in rock analysis, and a brand new combustible ice observation method is provided. Nuclear Magnetic Resonance (NMR) phenomenon was independently discovered by Bloch of Stanford university and Purcell et al of Harvard university in 1946, and was soon applied in the fields of physics, chemistry, material science, life science, medicine, and the like. With the increasing maturity of nuclear magnetic resonance technology, researchers find that it can be well applied to the research of combustible ice. The rapid response of nuclear magnetic resonance supports the condition of obtaining data in a sufficiently short time. In addition, through the nuclear magnetic resonance technology, the problems of compaction of the combustible ice sample, pore size requirements and the like do not exist. After the measurement, the sample was free of any damage. The combustible ice sample after nuclear magnetic resonance measurement can be subjected to other destructive experiments, so that the utilization rate of the sample is greatly improved. Also, the combustible ice samples retained their intact character until other experiments were performed. This also provides a guarantee for the accuracy of other experiments.

At present, the research on the decomposition rate of combustible ice is relatively small, and the research on instruments capable of accurately controlling the pressure condition of the combustible ice is also relatively small. When the nuclear magnetic resonance of a sample is measured, the constant pressure environment of the combustible ice cannot be ensured in most cases. In designing a pressure control device, it is important that the accuracy of the device be high enough. In measurements using nuclear magnetism, it is also considered whether experimental measurements have an effect on the proper functioning of the instrument. Therefore, the system for measuring the decomposition rate of the combustible ice provided by the application utilizes the constant pressure device in the system to provide a constant pressure condition, and researches the decomposition rate of the combustible ice through the rapid observation characteristic of nuclear magnetic resonance under the pressure stable condition.

As shown in FIG. 1, the system for measuring the decomposition rate of combustible ice provided by the application comprises a sample holder and a constant pressure device, wherein the constant pressure device comprises a pump 11, a pressure gauge 12, a liquid collecting device 13, a first back pressure valve 14 and an overflow liquid tank. As shown in fig. 2, the sample holder includes a fitting 21, a radio frequency coil 22, a pierced tube 23, a housing 24, a sample chamber 25, and a cooling liquid flow chamber 26. The sample holder forms a cylindrical holder by means of the fitting 21, the radio frequency coil 22, the pierced tube 23, the housing 24 and the sample chamber 25.

A cooling liquid flowing cavity 26 is arranged in a shell 24 of the sample holder, a closed sample cavity 25 is arranged in the cooling liquid flowing cavity 26, a hollow tube 23 is sleeved on the surface of the sample cavity 25, and a radio frequency coil 22 is wound on the hollow tube 23. The pump control fluid flows from an overflow tank to a first port of the sample holder, out of a second port of the sample holder after passing through the hollow tube 23 in the sample holder, through the first back pressure valve 14 into the liquid collection device 13.

It should be noted that all parts of the sample holder (except the coil) do not generate a nuclear magnetic signal in the magnetic field. The sample holder can be used under low temperature and high pressure conditions and can provide a relatively stringent temperature environment.

The hollow tube 23 and the radio frequency coil 22 form a whole and are assembled on the sample holder to form a whole, so that the problem that the radio frequency coil is added outside the sample holder to measure is avoided. The sample holder and the radio frequency coil form an integrated structure, so that the radio frequency coil only measures signals of the middle sample cavity 25 and the combustible ice sample, and noise generated by other parts can be greatly reduced. Therefore, the device space is saved, redundant noise caused by separation of the radio frequency coil and the sample holder is avoided, the nuclear magnetic resonance analyzer can obtain more accurate data, and the rule of analyzing the decomposition of the combustible ice is facilitated.

As shown in fig. 1, the system for measuring the decomposition rate of combustible ice further includes: the constant temperature device is used for controlling the temperature of the sample holder and comprises a cold water bath device, a second back pressure valve, a limiting liquid tank, a syringe pump and a heating bath device; the first end of the cooling liquid flowing cavity is connected with the first port of the cooling liquid bath device, a pressure gauge is arranged between the first port of the sample holder and the cooling liquid bath device, the second port of the cooling liquid bath device is connected with the first port of the limiting liquid tank, a pressure gauge and a second back pressure valve are arranged between the second port of the cooling liquid bath device and the limiting liquid tank, the second port of the limiting liquid tank is connected with the first port of the injection pump, the second port of the injection pump is connected with the first port of the heating liquid bath device, and the second port of the heating liquid bath device is connected with the second end of the cooling liquid flowing cavity. All parts of the constant temperature device are connected through pipelines, and the outer side of each pipeline can be wrapped with heat insulation materials. The cooling liquid flows out from the first end of the cooling liquid flowing cavity, sequentially flows through the cold water bath device, the second back pressure valve, the limiting liquid tank, the injection pump and the heating bath device, and flows into the second end of the cooling liquid flowing cavity.

Alternatively, the sample cavity in the sample holder may be made of a non-ferromagnetic (non-hydrogen non-magnetic) material to meet the requirements of the nuclear magnetic resonance cavity material.

Alternatively, a line leak in the environment may exchange heat with air causing a change in fluid temperature. Temperature is also an important factor affecting the phase change of combustible ice, so that a sufficiently thick layer of insulating material (e.g., aerogel, fiberglass, etc.) is required to be wrapped around the pipeline.

Alternatively, the constant pressure device pump may employ a plunger pump, such as an ISCO high pressure high precision plunger pump, with high precision flow rate and pressure control. By adjusting the pressure of the pump, fluid is forced into the sample holder.

Alternatively, the entire constant pressure device is sealed to a sufficient degree to withstand high pressure conditions, and therefore, stainless steel may be used as the material for the line.

Alternatively, pumping the fluid requires no signal to be generated in the nuclear magnetic instrument and is not susceptible to phase change under cryogenic conditions. In the embodiment of the present application, the flowing liquid outside the sample holder cavity may be selected from nitrogen (or other fluid meeting the requirement) which does not physically and chemically react with the combustible ice.

Based on the system for measuring the decomposition rate of the combustible ice, the method for measuring the decomposition rate of the combustible ice specifically comprises the following steps:

step 101: and putting the combustible ice sample into the sample cavity of the sample holder, and controlling the combustible ice sample not to have phase change by using the constant-pressure device.

Step 102: and measuring the transverse magnetization vector of the combustible ice sample by a nuclear magnetic resonance analyzer, and controlling the constant-voltage device until the transverse magnetization vector of the combustible ice sample is not changed.

Step 103: and determining the decomposition rate of the combustible ice sample according to the transverse magnetization vector and time of the combustible ice sample.

Optionally, prior to step 101, the sample holder is temperature stabilized by circulating a fluid outside the cavity of the sample holder. The method has the advantages that the stabilizing condition is not specifically limited, longer time is consumed when the temperature is more stable, and the time is short when the temperature precision requirement is low. A constant temperature is ensured by adjusting the temperature of the circulating fluid outside the cavity of the sample holder. By adjusting the temperature of the fluid in the cold and hot baths, the fluid is brought into contact with the internal pipeline, whereby the temperature of the circulating fluid inside the pipeline can be changed. At a constant temperature, the combustible ice changes phase once its pressure condition changes.

Optionally, in step 101, placing a combustible ice sample into a sample holder, opening a constant pressure device for pressure control, and controlling the transverse magnetization vector of the combustible ice sample not to change by using the constant pressure device; and in a long enough time, the pressure of the sample cavity is constant, and the combustible ice does not change the phase.

Alternatively, in step 102, the transverse magnetization vector of the combustible ice sample is measured by a nuclear magnetic resonance analyzer, and by controlling the pressure of the constant pressure device, as shown in fig. 3, the combustible ice is decomposed as the pressure is lower and lower. It should be noted that it is within the scope of the embodiments of the present application to control the pressure of the constant pressure device to be higher and higher, but the higher and higher pressure makes the formation process of the combustible ice difficult to control.

By setting relevant parameters of a nuclear magnetic resonance analyzer, the change of the transverse magnetization vector is continuously measured, the combustible ice sample is subjected to phase change through the change of pressure until the transverse magnetization vector of the combustible ice sample does not change after a preset time, the decomposition of the combustible ice sample is finished, and a curve graph of the transverse magnetization vector changing along with time can be obtained, as shown in fig. 4. By observing the dot pattern of the change of the transverse magnetization vector with time, the decomposition rate of combustible ice can be obtained. The plot is a plot of content versus time, and the combustible ice decomposition rate is equal to the content divided by the time.

In summary, the embodiment of the present application provides a system for measuring a decomposition rate of combustible ice, which includes a sample holder and a constant pressure device, wherein the constant pressure device includes a pump, a pressure gauge, a liquid collecting device, a first back pressure valve and an overflow liquid tank; the sample holder comprises a shell, a cooling liquid flowing cavity is arranged in the shell, a closed sample cavity is arranged in the cooling liquid flowing cavity, a hollow pipe is sleeved on the surface of the sample cavity, and a radio frequency coil is wound on the hollow pipe; the pump control fluid flows out from the overflow liquid tank to the inflow end of the cooling liquid flowing cavity, flows out from the outflow end of the cooling liquid flowing cavity after passing through the hollow pipe in the cooling liquid flowing cavity, and flows into the liquid collecting device through the first back pressure valve. Based on a system for measuring the decomposition rate of combustible ice, the constant-pressure device is controlled until the combustible ice sample does not change phase, then the nuclear magnetic resonance analyzer is used for measuring the transverse magnetization vector of the combustible ice sample, and the constant-pressure device is controlled until the transverse magnetization vector of the combustible ice sample does not change; so as to determine the decomposition rate of the combustible ice sample according to the change of the transverse magnetization vector of the combustible ice sample along with time.

The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. A system for measuring the decomposition rate of combustible ice is characterized by comprising a sample holder and a constant pressure device, wherein the constant pressure device comprises a pump, a pressure gauge, a liquid collecting device, a first back pressure valve and an overflow liquid tank; the sample holder comprises a shell, a cooling liquid flowing cavity is arranged in the shell, a closed sample cavity is arranged in the cooling liquid flowing cavity, a hollow pipe is sleeved on the surface of the sample cavity, and a radio frequency coil is wound on the hollow pipe;
the pump control fluid flows from an overflow fluid tank to a first port of the sample holder, out a second port of the sample holder after passing through the hollow tube in the sample holder, through the first back pressure valve, and into the liquid collection device.
2. The system of claim 1, wherein the system further comprises: the constant temperature device is used for controlling the temperature of the sample holder and comprises a cold water bath device, a second back pressure valve, a limiting liquid tank, a syringe pump and a heating bath device; all parts of the constant temperature device are connected through pipelines; the first end of the cooling liquid flowing cavity is connected with the first port of the cooling liquid bath device, a pressure gauge is arranged between the first port of the sample holder and the cooling liquid bath device, the second port of the cooling liquid bath device is connected with the first port of the limiting liquid tank, a pressure gauge and a second back pressure valve are arranged between the second port of the cooling liquid bath device and the limiting liquid tank, the second port of the limiting liquid tank is connected with the first port of the injection pump, the second port of the injection pump is connected with the first port of the heating liquid bath device, and the second port of the heating liquid bath device is connected with the second end of the cooling liquid flowing cavity;
the cooling liquid flows out from the first end of the cooling liquid flowing cavity, sequentially flows through the cold water bath device, the second back pressure valve, the limiting liquid tank, the injection pump and the heating bath device, and flows into the second end of the cooling liquid flowing cavity.
3. The system of claim 2, wherein the outside of the pipeline is wrapped with insulation.
4. The system of claim 1, wherein the fluid is nitrogen.
5. The system of claim 1, wherein the pump is a plunger pump.
6. The system of claim 1, wherein the sample chamber cavity of the sample holder is of a non-ferromagnetic material.
7. A method of measuring a decomposition rate of combustible ice using the system for measuring a decomposition rate of combustible ice according to any one of claims 1 to 6, comprising:
putting the combustible ice sample into a sample cavity of a sample holder, and controlling the combustible ice sample not to generate phase change by using a constant-pressure device;
measuring a magnetic resonance signal of the combustible ice sample;
and determining the decomposition rate of the combustible ice sample according to the magnetic resonance signal of the combustible ice sample.
8. The method of measuring a decomposition rate of combustible ice according to claim 7, wherein controlling the combustible ice sample from phase change using a constant pressure device comprises: controlling the transverse magnetization vector of the combustible ice sample to be unchanged by using the constant-voltage device;
the measuring of the magnetic resonance signal of the combustible ice sample comprises: measuring a transverse magnetization vector of the combustible ice sample by a nuclear magnetic resonance analyzer;
determining a decomposition rate of the combustible ice sample from the magnetic resonance signal of the combustible ice sample, comprising: and determining the decomposition rate of the combustible ice sample according to the change of the transverse magnetization vector of the combustible ice sample along with time.
9. The method of measuring a decomposition rate of combustible ice according to claim 8, wherein controlling the transverse magnetization vector of the combustible ice sample from changing by the constant voltage device comprises:
and controlling the pressure of the constant pressure device to enable the combustible ice sample to have phase change until the transverse magnetization vector of the combustible ice sample does not change after a preset time.
10. The method of measuring a decomposition rate of combustible ice according to claim 7, further comprising, prior to said placing a combustible ice sample into said sample holder:
a thermostatic device stabilizes the sample holder temperature by circulating a liquid outside the sample chamber body of the sample holder.
CN201811636313.0A 2018-12-29 2018-12-29 System and method for measuring decomposition rate of combustible ice CN111380892A (en)

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