CN110118678B - Natural gas hydrate-containing soil sample preparation equipment and sample preparation method thereof - Google Patents
Natural gas hydrate-containing soil sample preparation equipment and sample preparation method thereof Download PDFInfo
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- CN110118678B CN110118678B CN201910317293.9A CN201910317293A CN110118678B CN 110118678 B CN110118678 B CN 110118678B CN 201910317293 A CN201910317293 A CN 201910317293A CN 110118678 B CN110118678 B CN 110118678B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
- G01N2001/387—Other diluting or mixing processes mixing by blowing a gas, bubbling
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Abstract
The invention discloses a natural gas hydrate-containing soil sample preparation device and a sample preparation method thereof, wherein the device comprises a soil-ice powder mixture, and further comprises a reaction kettle, a freezing chamber, a hydraulic pump, a buffer container, a cylinder, a piston rod, a vacuum pump, a gas cylinder, a coil pipe, a cold bath, a flange, a pressure reducing valve, a ball valve, a first stop valve, a second stop valve, a third stop valve, a fourth stop valve, a fifth stop valve, a tee joint and a four-way joint. The invention integrates mixing, reacting, compacting and storing into a whole by improving the procedure of 'compacting first and then generating hydrate by the ice seed method', solves the problem of difficult air intake, avoids low-temperature operation, and completely carries out the sample preparation process in the environment of controllable temperature and pressure so as to reduce the adverse effect of uncontrollable factors on the sample preparation effect and can obtain a uniform natural gas-containing hydrated soil sample with definite components.
Description
Technical Field
The invention relates to the field of natural gas hydrate testing, in particular to a soil sample preparation device containing natural gas hydrate and a sample preparation method thereof.
Background
The mechanical test of the indoor artificially prepared natural gas hydrate-containing soil sample is an important means for researching the mechanical behavior of the natural gas hydrate-containing soil, so that the preparation of the sample with a decisive effect on the test result is particularly important.
At present, the method for artificially preparing the natural gas hydrate-containing soil comprises an unsaturated method, a gas dissolving method, an ice seed method and a hydrate pre-mixing method, wherein the former three methods are all used for generating hydrates in a soil sample, and the latter is used for mixing and pressing hydrate powder and soil into a sample; the ice seed method utilizes ice powder as a reactant to realize uniform generation of hydrate, but the problem of difficult air intake is still not solved, and the method is more prominent in fine soil; in the process of preparing the sample by the hydrate premixing method, the hydrate is easy to decompose, and the effect of preparing the sample is affected.
The unsaturated method is adopted by the institute of science and technology of China, the sequence of the generation of the hydrate at different parts of the sample is controlled by setting the gradient of the salt content and the temperature in the sample, so that the aim of generating uniform samples is fulfilled, but how to determine the gradient of the salt content and the temperature is a difficulty of the method; the university of Constipation and Qingdao marine geology institute adopts a hydrate premixing method to prepare samples, and in order to reduce the decomposition of the hydrate, the mixing and pressing processes of the samples are carried out at the low temperature of minus 10 ℃; preparing a sample by adopting ice seeds by Japanese high-grade industrial technical institute, mixing and pressing a soil-ice powder mixture at about-10 ℃, and then placing the mixture into a reaction kettle to generate a sample containing hydrated soil; the low temperature environment affects operators, and the sample preparation efficiency is too low.
In the mechanical test of the hydrated soil, the uniformity of a sample, the determination of the content of hydrate and the repeatability of the sample preparation directly influence the reliability of a test result, and compared with the sample preparation methods, the invention provides the hydrated soil sample preparation equipment, which improves the procedure of firstly compacting and then reacting to generate hydrate by an ice seed method, integrates mixing, reacting, compacting and storing, solves the problem of difficult air intake, avoids low-temperature operation and furthest reduces the influence of uncontrollable factors in the sample preparation process.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a natural gas hydrate-containing soil sample preparation device and a sample preparation method thereof, improves the procedure of 'firstly pressing and forming and then reacting to generate hydrate' by an ice seed method, integrates mixing, reacting, pressing and storing, solves the problem of difficult air intake, avoids low-temperature operation, and avoids adverse effect of uncontrollable factors of manual operation on sample preparation effect by the environment of controllable temperature and pressure, and can obtain uniform and definite-component natural gas hydrate-containing soil samples.
In order to solve the technical problems, the invention provides the following technical scheme:
The invention discloses a sample preparation device containing natural gas hydrate soil, which comprises a soil-ice powder mixture, a reaction kettle, a freezing chamber, a hydraulic pump, a buffer container, a cylinder, a piston rod, a vacuum pump, a gas cylinder, a coil, a cold bath, a flange, a pressure reducing valve, a ball valve, a first stop valve, a second stop valve, a third stop valve, a fourth stop valve, a fifth stop valve, a tee joint and a four-way valve, wherein the reaction kettle is communicated with the freezing chamber through the flange and the ball valve, the cylinder is connected with the piston through the piston rod, the flange is arranged at the top end of the reaction kettle, the bottom end of the reaction kettle is connected with the tee joint through a pipeline, the tee joint is connected with the four-way valve through a pipeline, the first stop valve is arranged on the pipeline between the tee joint and the four-way valve, the top end of the vacuum pump is connected with the four-way valve through the pipeline, the top end of the buffer container is connected with the four-way valve through the pipeline, the pressure reducing valve is connected with the gas cylinder through the four-way valve, the pressure reducing valve is connected with the four-way valve is connected with the upper end of the four-way valve through the pipeline, the end of the buffer container is connected with the outer surface of the pipeline, and the buffer container is wound on the outer surface of the pipeline, and the end of the buffer container is connected with the pipeline is formed by the side of the pipeline, and the buffer container is connected with the end is wound on the pipeline.
As a preferable technical scheme of the invention, the freezing chamber comprises an upper cover, a lower bottom and a cavity, wherein the upper cover and the lower bottom are made of steel materials, the cavity is made of organic glass, and a plurality of small holes for filling liquid nitrogen are formed in the cavity along a hollow sample hole.
As a preferable technical scheme of the invention, the top end of the buffer container is respectively connected with a pressure gauge and a thermometer.
As a preferable technical scheme of the invention, the inner diameters of the reaction kettle, the freezing chamber and the ball valve are the same, the diameter of the piston is smaller than 0.1mm of the inner diameters of the reaction kettle and the freezing chamber, and the end part of the piston is provided with a sealing ring.
As a preferable technical scheme of the invention, the cold bath is a low-temperature constant-temperature water tank.
The invention also correspondingly provides a sample forming method based on the natural gas hydrate-containing soil sample preparing equipment, which comprises the following steps of:
A. filling the soil-ice powder mixture into a reaction kettle; connecting a reaction kettle with a flange and a three-way valve; opening a cold bath, and cooling the reaction kettle; the cold bath is connected with the coil pipe in a reflux way, so that the reaction kettle is always kept in a cooling state from the step A;
B. Starting a vacuum pump, opening a first stop valve, a second stop valve and a ball valve, closing a third stop valve and a fifth stop valve, and vacuumizing the reaction kettle, the buffer container, the freezing chamber and the pipeline;
C. Opening the air cylinder to push the piston into the reaction kettle, and then closing the air cylinder;
D. Closing the first stop valve, the second stop valve and the fourth stop valve, opening the third stop valve, opening the pressure reducing valve and filling methane gas into the buffer container;
E. closing the third stop valve, opening the first stop valve and the fourth stop valve, filling methane gas into the reaction kettle, and stirring the soil-ice powder mixture by using high-speed air flow;
F. starting a hydraulic pump, setting output pressure, opening a fifth stop valve, and pressurizing methane gas in a buffer container;
G. regulating the temperature of the cold bath to 0 ℃, and enabling the ice powder and methane gas to react in the reaction kettle to generate hydrate;
H. closing the first stop valve, opening the fourth stop valve, opening the cylinder, and pressing the sample to a preset size;
I. closing a fourth stop valve, opening a first stop valve, regulating the pressure of a hydraulic pump, starting a cylinder at the same time, driving a piston and a sample into a freezing chamber, closing a ball valve, wherein the end part of the piston is positioned above the freezing chamber, injecting liquid nitrogen into a cavity of the freezing chamber, and disconnecting a flange;
J. Opening the ball valve, opening the cylinder, pushing the sample out of the freezing chamber, and taking out the prepared sample.
As a preferable technical scheme of the invention, the method for determining the hydrate content of the prepared sample comprises the following steps:
(1) At the end of step D, the readings of the pressure gauge and the thermometer are recorded, and the molar quantity of methane gas contained in the buffer container is calculated according to the Redlich-Kwong equation:
(2) G, recording the readings of the pressure gauge and the thermometer again at the end of the step G, and calculating the molar quantity of methane gas contained in the buffer container according to a Redlich-Kwong equation;
(3) And subtracting the molar quantity of the methane gas obtained by calculation to obtain the molar quantity of methane contained in the methane hydrate, namely the molar quantity of the methane hydrate.
Compared with the prior art, the invention has the following beneficial effects:
The invention integrates mixing, reacting, compacting and storing into a whole by improving the procedure of 'compacting first and then generating hydrate by the ice seed method', solves the problem of difficult air intake, avoids low-temperature operation, and completely carries out the sample preparation process in the environment of controllable temperature and pressure so as to reduce the adverse effect of uncontrollable factors on the sample preparation effect and can obtain a uniform natural gas-containing hydrated soil sample with definite components.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a schematic diagram of the overall structure of the present invention;
FIG. 2 is a schematic structural view of a reaction kettle according to the present invention;
FIG. 3 is a structural elevation of the freezing chamber of the present invention;
FIG. 4 is a cross-sectional view of a freezing chamber of the present invention;
FIG. 5 is a bottom view of an upper cover of the freezing chamber of the present invention;
FIG. 6 is a top view of the lower bottom of the freezer compartment of the present invention;
In the figure: 1. a soil-ice powder mixture; 2. a reaction kettle; 3. a flange; 4. a ball valve; 5. a freezing chamber; 6. a cylinder; 7. a piston; 71. a piston rod; 8. a hydraulic pump; 9. a buffer container; 10. a vacuum pump; 11. a gas cylinder; 12. a pressure gauge; 13. a thermometer; 14. a pressure reducing valve; 15. a first stop valve; 16. a second shut-off valve; 17. a third stop valve; 18. a fourth shut-off valve; 19. a fifth shut-off valve; 20. a coiled pipe; 21. cold bath; 22. an upper cover; 23. a lower bottom; 24. a cavity; 25. a tee joint; 26. a four-way joint.
Detailed Description
The preferred embodiments of the present invention will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present invention only, and are not intended to limit the present invention.
Example 1
As shown in fig. 1 to 6, the invention provides a natural gas hydrate-containing soil sample preparation device, which comprises a soil-ice powder mixture 1, and further comprises a reaction kettle 2, a freezing chamber 5, a hydraulic pump 8, a buffer container 9, a cylinder 6, a piston 7, a piston rod 71, a vacuum pump 10, a gas cylinder 11, a coil 20, a cold bath 21, a flange 3, a pressure reducing valve 14, a ball valve 4, a first stop valve 15, a second stop valve 16, a third stop valve 17, a fourth stop valve 18, a fifth stop valve 19, a tee joint 25 and a four-way 26, wherein the reaction kettle 2 and the freezing chamber 5 are communicated through the flange 3 and the ball valve 4, the cylinder 6 and the piston 7 are connected through the piston rod 71, the flange 3 is arranged at the top end of the reaction kettle 2, the bottom end of the reaction kettle 2 is connected with the tee joint 25 through a pipeline, the tee joint 25 is connected with the four-way valve 26 through the pipeline, the first stop valve 15 is arranged on a pipeline between the tee joint 25 and the four-way valve 26, the top of the vacuum pump 10 and the four-way valve 26 are connected through the pipeline, the second stop valve 16 is arranged on the pipeline between the vacuum pump 10 and the four-way valve 26, the top end of the buffer container 9 and the four-way valve 26 is connected with the pipeline 11 and the four-way valve 9 through the pipeline 11 and the pipeline 9, the pipeline 9 and the four-way valve 26 are connected to the end of the buffer container 9 through the pipeline 9 and the end of the buffer container 20 through the pipeline 9, the pipeline 9 is connected to the end of the three-way valve 2 and the end between the buffer container 2 and the end through the pipeline, which is connected to the pipeline 9 and the three-way valve through the pipeline, the pipeline is connected through the pipeline, the pipeline between the pipeline 2 and the pipeline is connected through the pipeline, the pipeline between the pipeline and the pipeline between the pipeline is connected between the valve and the four, and the valve 20 and the four.
The freezing chamber 5 comprises an upper cover 22, a lower bottom 23 and a cavity 24, the upper cover 22 and the lower bottom 23 are made of steel materials, the cavity 24 is made of organic glass, a plurality of small holes for filling liquid nitrogen are formed in the cavity 24 along a hollow sample hole, the sample hole in the center is convenient for a sample in the reaction kettle 2 to move upwards along with the piston 7 under the action of air pressure, the sample enters the freezing chamber 5 through the sample hole, and the small holes around the sample hole can be filled with the liquid nitrogen.
The top of the buffer container 9 is respectively connected with a pressure gauge 12 and a temperature gauge 13, so that the pressure and the temperature inside the buffer container 9 can be respectively displayed, and the pressure and the temperature can be conveniently observed and obtained in real time.
The internal diameters of the reaction kettle 2, the freezing chamber 5 and the ball valve 4 are the same, the diameter of the piston 7 is smaller than 0.1mm of the internal diameters of the reaction kettle 2 and the freezing chamber 5, and the sealing ring is arranged at the end part of the piston 7, so that the piston 7 can conveniently perform up-and-down telescopic movement in the reaction kettle 2 and the freezing chamber 5 without influencing the sealing effect.
The cold bath 21 is a low-temperature constant-temperature water tank which is an existing product on the market and is used for ensuring that the reaction kettle 2 is always in a low-temperature state.
The invention also correspondingly provides a sample forming method based on the natural gas hydrate-containing soil sample preparing equipment, which comprises the following steps of:
A. Filling the soil-ice powder mixture 1 into a reaction kettle 2; connecting the reaction kettle 2 with a flange 4 and a three-way valve 25; opening a cold bath 21 to cool the reaction kettle 2; the cold bath 21 is connected with the coil pipe 20 in a reflux way, so that the reaction kettle 2 is always kept in a cooling state from the step A;
B. Starting a vacuum pump 10, opening a first stop valve 15, a second stop valve 16 and a ball valve 4, closing a third stop valve 17 and a fifth stop valve 19, and vacuumizing the reaction kettle 2, the buffer container 9, the freezing chamber 5 and the pipeline;
C. opening the cylinder 6 to push the piston 7 into the reaction kettle 2, and then closing the cylinder 6;
D. Closing the first stop valve 15, the second stop valve 16 and the fourth stop valve 18, opening the third stop valve 17, opening the pressure reducing valve 14, and filling methane gas into the buffer container 9;
E. Closing the third stop valve 17, opening the first stop valve 15 and the fourth stop valve 18, filling methane gas into the reaction kettle 2, and stirring the soil-ice powder mixture 1 by using high-speed airflow;
F. Opening the hydraulic pump 8, setting output pressure, opening the fifth stop valve 19, and pressurizing methane gas in the buffer container 9;
G. Regulating the temperature of the cold bath 21 to 0 ℃, and enabling the ice powder and methane gas to react in the reaction kettle 2 to generate hydrate;
H. closing the first stop valve 15, opening the fourth stop valve 18, opening the cylinder 6, and pressing the sample to a predetermined size;
I. closing a fourth stop valve 18, opening a first stop valve 15, increasing the pressure of the hydraulic pump 8, simultaneously starting the cylinder 8, driving the piston 7 and the sample into the freezing chamber 5, closing the ball valve 4, wherein the end part of the piston 7 is positioned above the freezing chamber 5, injecting liquid nitrogen into the cavity of the freezing chamber 5, and disconnecting the flange 3;
J. the ball valve 4 is opened, the cylinder 6 is opened, the sample is pushed out of the freezing chamber 5, and the prepared sample is taken out.
The method for determining the hydrate content of the prepared sample is as follows:
(1) At the end of step D, the readings of the pressure gauge 12 and of the thermometer 13 are recorded, and the molar quantity of methane gas contained in the buffer vessel is calculated according to the Redlich-Kwong equation:
(2) At the end of the step G, the readings of the pressure gauge 12 and the thermometer 13 are recorded again, and the molar quantity of methane gas contained in the buffer container is calculated according to a Redlich-Kwong equation;
(3) And subtracting the molar quantity of the methane gas obtained by calculation to obtain the molar quantity of methane contained in the methane hydrate, namely the molar quantity of the methane hydrate.
Specifically, firstly, opening a flange 4, and filling the soil-ice powder mixture 1 into a reaction kettle 2; connecting the reaction kettle 2 with a flange 4 and a three-way valve 25; opening a cold bath 21 to cool the reaction kettle 2; the cold bath 21 is connected with the coil pipe 20 in a reflux way, so that the reaction kettle 2 is always kept in a cooling state from the step A; starting a vacuum pump 10, opening a first stop valve 15, a second stop valve 16 and a ball valve 4, closing a third stop valve 17 and a fifth stop valve 19, and vacuumizing the reaction kettle 2, the buffer container 9, the freezing chamber 5 and the pipeline; opening the cylinder 6 to push the piston 7 into the reaction kettle 2, and then closing the cylinder 6; closing the first stop valve 15, the second stop valve 16 and the fourth stop valve 18, opening the third stop valve 17, opening the pressure reducing valve 14, and filling methane gas into the buffer container 9; closing the third stop valve 17, opening the first stop valve 15 and the fourth stop valve 18, filling methane gas into the reaction kettle 2, and stirring the soil-ice powder mixture 1 by using high-speed airflow; opening the hydraulic pump 8, setting output pressure, opening the fifth stop valve 19, and pressurizing methane gas in the buffer container 9; regulating the temperature of the cold bath 21 to 0 ℃, and enabling the ice powder and methane gas to react in the reaction kettle 2 to generate hydrate; closing the first stop valve 15, opening the fourth stop valve 18, opening the cylinder 6, and pressing the sample to a predetermined size; closing a fourth stop valve 18, opening a first stop valve 15, increasing the pressure of the hydraulic pump 8, simultaneously starting the cylinder 8, driving the piston 7 and the sample into the freezing chamber 5, closing the ball valve 4, wherein the end part of the piston 7 is positioned above the freezing chamber 5, injecting liquid nitrogen into the cavity of the freezing chamber 5, and disconnecting the flange 3; the ball valve 4 is opened, the cylinder 6 is opened, the sample is pushed out of the freezing chamber 5, and the prepared sample is taken out.
Compared with the prior art, the invention has the following beneficial effects:
The invention integrates mixing, reacting, compacting and storing into a whole by improving the procedure of 'compacting first and then generating hydrate by the ice seed method', solves the problem of difficult air intake, avoids low-temperature operation, and completely carries out the sample preparation process in the environment of controllable temperature and pressure so as to reduce the adverse effect of uncontrollable factors on the sample preparation effect and can obtain a uniform natural gas-containing hydrated soil sample with definite components.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A sample preparation method based on a sample preparation device containing natural gas hydrate soil comprises sample preparation equipment, wherein the sample preparation equipment comprises a reaction kettle (2), a freezing chamber (5), a hydraulic pump (8), a buffer container (9), a cylinder (6), a piston (7), a piston rod (71), a vacuum pump (10), a gas cylinder (11), a coil pipe (20), a cold bath (21), a flange (3), a pressure reducing valve (14), a ball valve (4), a first stop valve (15), a second stop valve (16), a third stop valve (17), a fourth stop valve (18), a fifth stop valve (19), a tee joint (25) and a four-way valve (26), wherein the reaction kettle (2) is communicated with the freezing chamber (5) through the flange (3) and the ball valve (4), the cylinder (6) is connected with the piston (7) through the piston rod (71), the flange (3) is arranged at the top end of the reaction kettle (2), the bottom end of the reaction kettle (2) is connected with the tee joint (25) through a pipeline, the tee joint (25) is connected with the tee joint (26) through the pipeline, the tee joint (25) is arranged between the tee joint (25) and the four-way joint (26) through the pipeline (10), the method is characterized in that the second stop valve (16) is arranged on a pipeline between the vacuum pump (10) and the four-way valve (26), the top end of the buffer container (9) is connected with the four-way valve (26) through the pipeline, the gas cylinder (11) and the four-way valve (26) are connected through the pipeline, the pressure reducing valve (14) and the third stop valve (17) are connected on the pipeline between the gas cylinder (11) and the four-way valve (26), the right end bottom of the buffer container (9) is connected with the three-way valve (25) through the pipeline, the fourth stop valve (18) is arranged on the pipeline between the buffer container (9) and the three-way valve (25), the left end bottom of the hydraulic pump (8) and the buffer container (9) are connected through the pipeline, the fifth stop valve (19) is arranged on the pipeline between the hydraulic pump (8) and the buffer container (9), the coil pipe (20) is wound on the outer surface of the reaction kettle (2), and the outer end of the coil pipe (20) is communicated with the cold bath (21) to form a loop, and the method comprises the following steps:
A. Filling the soil-ice powder mixture (1) into a reaction kettle (2); connecting the reaction kettle (2) with a flange (4) and a three-way valve (25); opening a cold bath (21) to cool the reaction kettle (2); the cold bath (21) is connected with the coil pipe (20) in a reflux way, so that the reaction kettle (2) is always kept in a cooling state from the step A;
B. Opening a vacuum pump (10), opening a first stop valve (15), a second stop valve (16) and a ball valve (4), closing a third stop valve (17) and a fifth stop valve (19), and vacuumizing the reaction kettle (2), the buffer container (9), the freezing chamber (5) and the pipeline;
C. Opening the air cylinder (6) to push the piston (7) into the reaction kettle (2), and then closing the air cylinder (6);
D. Closing the first stop valve (15), the second stop valve (16) and the fourth stop valve (18), opening the third stop valve (17), opening the pressure reducing valve (14) and filling methane gas into the buffer container (9);
E. Closing a third stop valve (17), opening a first stop valve (15), and a fourth stop valve (18), filling methane gas into the reaction kettle (2), and stirring the soil-ice powder mixture (1) by using high-speed air flow;
F. Opening a hydraulic pump (8), setting output pressure, opening a fifth stop valve (19), and pressurizing methane gas in a buffer container (9);
G. regulating the temperature of the cold bath (21) to 0 ℃, and enabling the ice powder and methane gas to react in the reaction kettle 2 to generate hydrate;
H. closing the first stop valve (15), opening the fourth stop valve (18), opening the cylinder (6), and pressing the sample to a predetermined size;
I. Closing a fourth stop valve (18), opening a first stop valve (15), increasing the pressure of the hydraulic pump (8), starting the cylinder (8) at the same time, driving the piston (7) and the sample into the freezing chamber (5), closing the ball valve (4), wherein the end part of the piston 7 is positioned above the freezing chamber (5), injecting liquid nitrogen into the cavity of the freezing chamber (5), and disconnecting the flange (3);
J. Opening the ball valve (4), opening the cylinder (6), pushing the sample out of the freezing chamber (5), and taking out the prepared sample.
2. The sampling method based on the natural gas hydrate-containing soil sampling equipment according to claim 1, wherein the freezing chamber (5) comprises an upper cover (22), a lower bottom (23) and a cavity (24), the upper cover (22) and the lower bottom (23) are made of steel materials, the cavity (24) is made of organic glass, and a plurality of small holes for filling liquid nitrogen are formed in the cavity (24) along a hollow sample hole.
3. The sampling method based on the natural gas hydrate-containing soil sampling equipment according to claim 1, wherein the top end of the buffer container (9) is respectively connected with a pressure gauge (12) and a thermometer (13).
4. The sample forming method based on the natural gas hydrate soil sample forming equipment according to claim 1, wherein the inner diameters of the reaction kettle (2), the freezing chamber (5) and the ball valve (4) are the same, the diameter of the piston (7) is smaller than the inner diameters of the reaction kettle (2) and the freezing chamber (5) by 0.1mm, and a sealing ring is arranged at the end part of the piston (7).
5. A method of forming a sample based on a natural gas hydrate-containing soil sampling apparatus according to claim 1, characterized in that the cold bath (21) is a cryogenic constant temperature water bath.
6. The method for forming a sample based on a natural gas hydrate-containing soil sample preparation device according to claim 1, wherein the method for determining the hydrate content of the prepared sample is as follows:
(1) At the end of step D, the readings of the pressure gauge (12) and the thermometer (13) are recorded, and the molar quantity of methane gas contained in the buffer container is calculated according to the Redlich-Kwong equation:
(2) G, recording the readings of the pressure gauge (12) and the thermometer (13) again at the end of the step G, and calculating the molar quantity of methane gas contained in the buffer container according to a Redlich-Kwong equation;
(3) And subtracting the molar quantity of the methane gas obtained by calculation to obtain the molar quantity of methane contained in the methane hydrate, namely the molar quantity of the methane hydrate.
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| CN110835566A (en) * | 2019-11-28 | 2020-02-25 | 中国石油大学(华东) | High-gas-content methane hydrate ball and preparation method thereof |
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