CN109991114B - Tetrahydrofuran hydrate-containing soil water retention parameter testing device and method thereof - Google Patents
Tetrahydrofuran hydrate-containing soil water retention parameter testing device and method thereof Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002689 soil Substances 0.000 title claims abstract description 23
- BSCHIACBONPEOB-UHFFFAOYSA-N oxolane;hydrate Chemical compound O.C1CCOC1 BSCHIACBONPEOB-UHFFFAOYSA-N 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 194
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 239000007789 gas Substances 0.000 claims abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 230000001105 regulatory effect Effects 0.000 claims abstract description 14
- 238000003860 storage Methods 0.000 claims abstract description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 78
- 239000000523 sample Substances 0.000 claims description 69
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 34
- 239000012530 fluid Substances 0.000 claims description 27
- 238000007789 sealing Methods 0.000 claims description 27
- 239000004927 clay Substances 0.000 claims description 18
- 229920001971 elastomer Polymers 0.000 claims description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 8
- 239000013049 sediment Substances 0.000 claims description 8
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000012774 insulation material Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000009738 saturating Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- 238000004781 supercooling Methods 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000013519 translation Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 description 6
- 239000000110 cooling liquid Substances 0.000 description 5
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 150000004677 hydrates Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a device and a method for testing water retention parameters of soil containing tetrahydrofuran hydrate, and relates to a technology for testing water retention parameters of soil containing tetrahydrofuran hydrate. The device comprises a testing part and a water bath constant temperature part; the test part comprises a high-pressure nitrogen bottle (1), a pressure reducing valve (2), a pressure regulating pump (3), pressure (4), a water storage bottle (5), a gas collecting tube (6), a liquid collecting cup (7), a balance (8), a data acquisition system (9) and 1 st to 3 rd valves (V1 to V3); the water bath constant temperature part comprises a constant temperature water bath box (10), a circulating pump (11), a temperature sensor (12), a refrigerating system (13) and 4 th to 7 th valves (V4 to V7). The invention can simply and quickly prepare uniform and stable soil sample containing hydrate; the SWCC curve can be simply, conveniently, quickly and accurately obtained; the suction range is wider, and the manual error of the traditional shaft translation method test can be reduced.
Description
Technical Field
The invention relates to a technology for testing water retention parameters of hydrate-containing soil, in particular to a device and a method for testing water retention parameters of Tetrahydrofuran (THF) -containing hydrate-containing soil.
Specifically, the method relates to measurement of a soil-water characteristic relation curve (SWCC) of tetrahydrofuran hydrate-containing soil under different hydrate content conditions, a sample is controlled to form tetrahydrofuran hydrate under a low-temperature condition and is tested, suction force is controlled and measured by utilizing an axis translation technology, the water yield of the sample is acquired and recorded according to a data automatic acquisition system, suction force balance is judged, the water content of the sample under the suction force is calculated, and the soil-water characteristic relation curve of tetrahydrofuran hydrate-containing soil under different hydrate content conditions is obtained, so that important data support is provided for hydrate exploitation.
Background
Natural gas hydrate is a novel clean energy source, but incorrect exploitation can cause engineering problems such as submarine landslide, ground collapse and the like, and greenhouse gases can be released to cause global warming. The water retention characteristic parameters of the hydrate-containing sediment are very important basic parameters in the drilling and exploitation process of the natural gas hydrate, and the mechanical property, the gas-water migration process and the occurrence state of the sediment are all related to the water retention property of the sediment. The soil-water characteristic relation curve (SWCC) is a relation curve between the water content and the suction force of the soil body, reflects the water holding capacity of the soil body, and is a key function for describing the behavior of unsaturated soil. SWCC curves are essentially determined by pore scale characteristics, including pore shape and size distribution, interconnectivity and spatial variability, fluid and interfacial tension, etc., and the presence of hydrates in the sediment can greatly alter the pore scale characteristics of the soil.
The development of the SWCC curve of the deposit containing the hydrate has great difficulty, and the high fluid pressure and low temperature condition required by the decomposition of the hydrate are avoided; meanwhile, long induction time is needed for synthesizing methane hydrate in a laboratory, the solubility of methane in water is low, seepage loss is large, the stability of a sample in a test is difficult, and the cost of synthesis and test equipment is high, so that related data is extremely deficient. Studies show that Tetrahydrofuran (THF) hydrate and methane hydrate have similar thermophysical properties, the above difficulties can be overcome, experimental study can be carried out by replacing methane hydrate, synthesis only needs to control low-temperature conditions, and the saturation of THF hydrate is easy to control, so that an indoor test device for testing the SWCC curve of the deposit of THF hydrate is developed by using THF hydrate as a test object. The device can overcome the defects of long time consumption, small suction range, error caused by periodic manual reading of test data, no temperature control system and the like of a common pressure plate method in soil-water characteristic relation curve test, and can be used for testing a SWCC curve of a THF hydrate sediment and a conventional sample.
At present, the device and the method for researching and testing the water retention parameters of the hydrate-containing soil are not reported yet through searching.
The invention comprises the following steps:
The invention aims to fill the blank of an indoor test device for acquiring the water retention parameter of a sediment containing hydrate at home and abroad, overcome the defects in the prior art, and provide the device and the method for testing the water retention parameter of the soil containing the tetrahydrofuran hydrate.
The invention adopts the technical proposal for solving the problems that:
The device applies air pressure to a sample in a pressure chamber by using nitrogen under a low temperature condition, controls and measures the suction force of the sample containing THF hydrate by using an axial translation method, judges the suction force balance and calculates the water content of the sample under the suction force according to the acquisition of the water yield of the sample by a data automatic acquisition system, obtains a soil-water characteristic curve (SWCC) of the soil containing THF hydrate, greatly shortens the test time, realizes the study of the water-holding parameter of the soil containing THF hydrate, and has the principle conforming to the hydrate formation mode and the exploitation working condition, simple structure and low cost, and can be used for most scientific research and design unit equipment.
The method comprises the steps of placing a sample in a tetrahydrofuran aqueous solution with a certain concentration for saturation, and placing the sample in a constant-temperature water bath for cooling and induction to obtain tetrahydrofuran-containing hydrated soil with uniformly distributed hydrates; the THF hydrate-containing sample is put on a clay plate in a pressure chamber of a constant-temperature water bath, various levels of air pressure are applied to the pressure chamber, the suction force of the THF hydrate-containing sample is controlled and measured by an axial translation method, a data acquisition system automatically acquires and records water yield data of the sample in the pressure chamber, the balance and the water content of the sample can be rapidly judged according to the water yield state, and a soil-water characteristic relation curve (SWCC) under different hydrate saturation conditions is obtained.
Specifically:
1. tetrahydrofuran-containing hydrate soil water retention parameter testing device
The device comprises a testing part and a water bath constant temperature part;
the test part comprises a high-pressure nitrogen bottle, a pressure reducing valve, a pressure regulating pump, a pressure chamber, a water storage bottle, a gas collecting pipe, a liquid collecting cup, a balance, a data acquisition system and 1 st to 3 rd valves;
the water bath constant temperature part comprises a constant temperature water bath box, a temperature sensor, a circulating pump, a refrigerating system and a 4 th to 7 th valve;
the positions and the connection relations are as follows:
a pressure chamber is arranged in the constant-temperature water bath box, and a sample and a clay plate which are connected up and down are arranged in the pressure chamber to provide a test place for the sample;
The high-pressure nitrogen cylinder, the pressure reducing valve and the pressure regulating pump are connected to an air inlet of the upper cover of the pressure chamber through pipelines in sequence to provide a pneumatic environment for the sample;
the water storage bottle, the 1 st valve and the water inlet of the pressure chamber are sequentially communicated to provide a hydraulic environment for the sample;
the water outlet of the pressure chamber, the 2 nd valve, the gas collecting pipe, the 3 rd valve and the liquid collecting cup are sequentially communicated, the liquid collecting cup is arranged on a balance, the balance is connected with a data acquisition system, and the change of the water outlet of the sample is measured;
The probes of the temperature sensor are arranged at the top, the middle and the bottom in the constant-temperature water bath box, the temperature sensor and the data acquisition system are connected, and the temperature of the surrounding environment of the sample is measured;
a heat conduction copper pipe is arranged in the constant-temperature water bath box, and a refrigerating fluid inlet, a water circulation inlet, a refrigerating fluid outlet and a water circulation outlet are respectively arranged on the left side wall and the right side wall of the constant-temperature water bath box;
The water circulation inlet, the 5 th valve V5 circulation pump, the 6 th valve and the water circulation outlet are sequentially communicated in a closed loop manner, so that a constant temperature environment is provided for the sample;
The outlet of the refrigerating system, the 4 th valve, the refrigerating fluid inlet, the heat conducting copper pipe, the refrigerating fluid outlet, the 7 th valve and the inlet of the refrigerating system are sequentially communicated in a closed loop manner, and a refrigerating environment is provided for the sample.
Working principle:
The device utilizes a water bath constant temperature system to control the temperature, a sample saturated by tetrahydrofuran solution with a certain concentration is subjected to cooling induction in the water bath constant temperature system, THF-containing hydrate samples with different hydrate contents and even distribution are quickly prepared, the THF-containing hydrate samples are placed on a clay plate in a pressure chamber, the pressure chamber is completely assembled in a constant temperature water bath box, a high-pressure nitrogen cylinder is used for applying air pressure at all levels to the pressure chamber, a pressure reducing valve can be used for changing high-pressure air in the nitrogen cylinder into low-pressure air to be conveyed to the pressure chamber, a pressure regulating pump can be used for pressurizing or relieving pressure, the air pressure in the pressure chamber is regulated, a water storage cylinder is used for carrying out saturation treatment on the whole system and enabling water to be filled in the whole test pipeline, a gas collecting pipe is used for collecting the gas in the pipeline in the test debugging stage to ensure that the collected liquid in the liquid collecting cup is discharged as the sample, the water mass of the sample is automatically read and recorded by a balance connected with a data collecting system, the balance and the water content can be quickly judged according to the water yield state, so that a Soil Water Characteristic Curve (SWCC) under different hydrate saturation conditions can be obtained.
The invention has the following advantages and positive effects:
1. the uniform and stable hydrated soil sample can be simply and quickly prepared;
2. The SWCC curve can be simply, conveniently, quickly and accurately obtained;
3. the suction range is wider, and the manual error of the traditional shaft translation method test can be reduced.
Drawings
FIG. 1 is a schematic diagram of the structure of the present device;
FIG. 2 is a schematic view of the structure of the pressure chamber;
FIG. 3 is a schematic view of the structure of the thermostatic waterbath.
Wherein:
1-a high-pressure nitrogen cylinder;
2-a pressure reducing valve;
3-a pressure regulating pump;
4-a pressure chamber, wherein the pressure chamber is provided with a pressure chamber,
4-1 Air inlet, 4-2-1 sealing rubber ring, 4-3 fixing screw,
4-Organic glass, 4-5-sample, 4-6-clay plate,
4-7 To 2 th sealing rubber ring, 4-8 to water outlet, 4-9 to water inlet,
4-10 Parts of pressure chamber base, 4-11 parts of pressure chamber upper cover and 4-12 parts of drainage groove;
5-a water storage bottle;
6, a gas collecting tube;
7, collecting liquid cup;
8-a balance;
9, a data acquisition system;
10-a constant-temperature water bath box,
10-1 Of water bath box upper cover, 10-2 of upper cover handle, 10-3 of water bath box body,
10-4 Parts of heat conduction copper pipe, 10-5 parts of refrigerating fluid inlet, 10-6 parts of water circulation inlet,
10-7-Refrigerating fluid outlet and 10-8-water circulation outlet;
11-a temperature sensor;
12-a circulation pump;
13-a refrigeration system;
V1, V2, V7-1 st and 2-7 th valves.
Detailed Description
1. Device and method for controlling the same
1. Overall (L)
As shown in fig. 1,2 and 3, the device comprises a testing part and a water bath constant temperature part;
The test part comprises a high-pressure nitrogen bottle 1, a pressure reducing valve 2, a pressure regulating pump 3, a pressure chamber 4, a water storage bottle 5, a gas collecting tube 6, a liquid collecting cup 7, a balance 8, a data acquisition system 9 and 1 st to 3 rd valves V1 to V3;
the water bath constant temperature part comprises a constant temperature water bath box 10, a temperature sensor 11, a circulating pump 12, a refrigerating system 13 and 4 th to 7 th valves V4 to V7;
1) Test part
The high-pressure nitrogen bottle 1, the pressure reducing valve 2 and the pressure regulating pump 3 are sequentially connected to an air inlet 4-1 of a pressure chamber upper cover 4-11 through pipelines, in order to better observe the condition of a sample 4-5, an organic glass cover 4-4 is used as the outer wall of the pressure chamber 4, the pressure chamber upper cover 4-11, the organic glass cover 4-4 and a pressure chamber base 4-10 are connected through three fixing screws 4-3, the upper edge of the organic glass cover 4-4 and the pressure chamber upper cover 4-11 are sealed through a1 st sealing rubber ring 4-2 and the pressure chamber base 4-10, the 2 nd sealing rubber ring 4-7 is also sealed and fixed with a ceramic plate 4-6, the sample 4-5 is arranged on the ceramic plate 4-6, a drain groove 4-12, a water outlet 4-8 and a water inlet 4-9 are arranged below the ceramic plate 4-6, the water inlet 4-9 is connected to the pressure chamber base 5 through a pipeline and a1 st valve V1, the water outlet 4-8 is connected to a water collecting pipe 6 through a pipeline and a2 nd valve V2, the water outlet 4-8 is connected to a water collecting pipe 6, the water collecting pipe 6 is connected to a balance system through a 3 rd valve V3 and a 6, the water collecting system is connected to a water collecting system through a2 nd valve V3, the water collecting system is drawn, the water volume is automatically and the water volume is drawn and data is recorded by a balance system, the water volume is automatically drawn and the water volume is drawn and is stored in a system.
2) Constant temperature part of water bath
The THF hydrate formation requires a low temperature environment, so the pressure chamber 4 in which the THF hydrate-containing samples 4 to 5 are placed in the test section is placed in a constant temperature water bath 10 for the test, and the refrigerating fluid is prepared from ethylene glycol and distilled water according to the ratio of 1:2, configuring; the constant-temperature water bath 10 consists of a box body 10-3 and an upper cover 10-1, wherein the upper cover 10-1 is formed by combining two small rectangular covers with connecting holes, so that the pressure chamber 4 is conveniently connected through a pipeline, a heat conduction copper pipe 10-4 is arranged in the box body 10-3 for cooling liquid circulation, the cooling liquid is cooled by a cooling system 13, the cooling liquid enters the heat conduction copper pipe 10-4 from a cooling liquid inlet 10-5 through a pipeline and a 4 th valve V4 of the cooling system 13, and returns to the cooling system 13 through a pipeline and a 7 th valve V7 of a cooling liquid outlet 10-7; in order to ensure that the temperature of water bath in the tank body 10-3 is uniform, a circulating pump 12 is arranged outside the water bath tank 10 for water circulation, and water in the tank body enters a water circulation inlet 10-6 from a water circulation outlet 10-8 through a pipeline, a 6 th valve V6, the circulating pump 12 and a5 th valve V5; in order to detect whether the temperature of the water bath 10 reaches the target temperature and the temperature is uniform, 3 temperature probes in the temperature sensor 11 are respectively arranged at the top, the middle and the bottom of the water bath 10, and data are automatically recorded on the data acquisition system 9.
The positions and the connection relations are as follows:
a pressure chamber 4 is arranged in the constant-temperature water bath 10, and a sample 4-5 and a clay plate 4-6 which are connected up and down are arranged in the pressure chamber 4 to provide a test place for the sample 4-5;
The high-pressure nitrogen bottle 1, the pressure reducing valve 2 and the pressure regulating pump 3 are connected to the air inlet 4-1 of the pressure chamber upper cover 4-11 through pipelines in sequence to provide a pneumatic environment for the sample 4-5;
The water storage bottle 5, the 1 st valve V1 and the water inlet 4-9 of the pressure chamber 4 are sequentially communicated to provide a water pressure environment for the sample 4-5;
the water outlet 4-8 of the pressure chamber 4, the valve V2 of the 2 nd valve, the gas collecting tube 6, the valve V3 of the 3 rd valve and the liquid collecting cup 7 are sequentially communicated, the liquid collecting cup 7 is arranged on the balance 8, the balance 8 and the data acquisition system 9 are connected, and the change of the water outlet of the sample 4-5 is measured;
probes of the temperature sensor 11 are respectively arranged at the top, the middle and the bottom in the constant-temperature water bath 10, the temperature sensor 11 is connected with the data acquisition system 9, and the temperature of the surrounding environment of the sample 4-5 is measured;
A heat conduction copper pipe 10-4 is arranged in the constant temperature water bath 10, and a refrigerating fluid inlet 10-5, a water circulation inlet 10-6, a refrigerating fluid outlet 10-7 and a water circulation outlet 10-8 are respectively arranged on the left side wall and the right side wall of the constant temperature water bath 10;
The water circulation inlet 10-6, the 5 th valve V5, the circulation pump 12, the 6 th valve V6 and the water circulation outlet 10-8 are sequentially communicated in a closed loop manner, so that a constant temperature environment is provided for the sample 4-5;
The outlet of the refrigerating system 13, the 4 th valve V4, the refrigerating fluid inlet 10-5, the heat conduction copper pipe 10-4, the refrigerating fluid outlet 10-7, the 7 th valve V4 and the inlet of the refrigerating system 13 are sequentially communicated in a closed loop manner, and a refrigerating environment is provided for the sample 4-5.
2. Functional component
1) High pressure nitrogen cylinder 1
Is a common nitrogen gas storage bottle provided by Guangdong south China special gas research all companies.
2) Pressure reducing valve 2
Selecting the product of Shanghai Weiyun Utility Co., ltd., model: YQY-12, 15MPa of input pressure and 0.1-1.25MPa of regulation range.
3) Pressure regulating pump 3
FAIRCHILD INDUSTRIAL PRODUCTS COMPANY products and models are selected: m30BP, adjustment range: 0-15kPa,15-700kPa, maximum pressure: 1000kpa, precision: 0.15psi.
4) Pressure chamber 4
As shown in FIG. 2, the pressure chamber 4 comprises an air inlet 4-1, a1 st sealing rubber ring 4-2, a fixing screw 4-3, an organic glass cover 4-4, a sample 4-5, a clay plate 4-6, a2 nd sealing rubber ring 4-7, a water outlet 4-8, a water inlet 4-9, a pressure chamber base 4-10 and an upper cover 4-11 number drainage groove 4-12;
the positions and the connection relations are as follows:
from bottom to top, the base 4-10, the organic glass cover 4-4 and the upper cover 4-11 are connected into a sealed container through 3 uniformly distributed fixing screws 4-3, and the joint is sealed by an O-shaped 1 st sealing rubber ring 4-2 and a 2 nd sealing rubber ring 4-7;
An air inlet 4-1 is arranged on the upper cover 4-11;
4-6 diameter of clay plate The 2 nd sealing rubber ring 4-7 is embedded at the top of the base 4-10, a sample 4-5 is arranged above the clay plate 4-6, and a drainage groove 4-12, a water outlet 4-8 and a water inlet 4-9 are arranged below the clay plate 4-6.
5) Water storage bottle 5
Is a common water storage bottle with the capacity of 2L.
6) Gas collecting tube 6
Is a common gas collecting tube with scales, the capacity is 15ml, and the precision is 0.5ml.
7) Liquid collecting cup 7
Is a common beaker with the capacity of 200ml, and is subjected to sealing treatment, and a small hole connecting pipeline is reserved at the cup opening.
8) Balance 8
Adopting an Ohaus brand electronic scale, and the model is as follows: scout pro SP202, weigh: 200g, precision: 0.01g.
9) Data acquisition system 9
Agilent data acquisition instrument and data acquisition software are selected, and the model is: 34972A, the balance 8 and the temperature sensor 11 are connected through a channel provided by the collector to collect data, record and process.
10 Constant temperature water bath 10)
As shown in FIG. 3, the constant temperature water bath 10 comprises a water bath upper cover 10-1, an upper cover handle 10-2, a water bath body 10-3, a heat conduction copper pipe 10-4, a refrigerating fluid inlet 10-5, a water circulation inlet 10-6, a refrigerating fluid outlet 10-7 and a water circulation outlet 10-8;
the positions and the connection relations are as follows:
the upper cover 10-1 of the water bath box and the upper and lower parts of the water bath box body 10-3 are connected into a whole;
An upper cover handle 10-2 is arranged on the upper cover 10-1 of the water bath box;
The upper part and the lower part in the water bath box body 10-3 are respectively provided with a heat conduction copper pipe 10-4;
The upper part of the inner wall of the water bath box body 10-3 is respectively provided with a refrigerating fluid inlet 10-5 and a water circulation inlet 10-6;
The lower part of the inner wall of the water bath box body 10-3 is respectively provided with a refrigerating fluid outlet 10-7 and a water circulation outlet 10-8.
(1) Water bath box upper cover 10-1
The two small rectangular covers with connecting holes are combined, the size is 40cm multiplied by 40cm, the thickness is 3cm, and the inside is filled with heat preservation and insulation materials; the opening size diameter d=4 cm.
(2) Upper cover handle 10-2
A common piece.
(3) Water bath box 10-3
The square container has the dimensions of 40cm multiplied by 50cm and the thickness of 3cm, and is internally filled with heat preservation and insulation materials.
Four drill holes are arranged: sealing the drilling hole wall, wherein the diameter d=1 cm is formed by a refrigerating fluid inlet 10-5, a water circulation inlet 10-6, a refrigerating fluid outlet 10-7 and a water circulation outlet 10-8.
(4) Heat conduction copper pipe 10-4
The common piece, 1/2 pipe, with an outer diameter of 12.7mm, is tightly attached to the spiral disc stack inside the box 10-3.
11 A) circulation pump 11
The Jiangsu blue instrument is selected to be manufactured into the products of the limited company, the model: BT-200B, dual-channel output, output flow: 2X (1-6800) ml/h, output pressure: more than or equal to 2.5kg/cm < 2 >.
12 Temperature sensor 12)
3 Beijing Sai Yiling Ling technology Co., ltd., product name: pt100, model: 1632-100, working temperature: -40-450 ℃, error: (+/-) (0.15+0.002|t|).
13 Refrigeration system 13)
Selecting a Ningbo Tianheng instrument factory low-temperature constant-temperature tank product, and the model: THD-2030, temperature range:
-20-100 ℃, and the control precision is as follows: a circulating pump is arranged in the reactor at 0.01 ℃ and the pump flow is 13L/min.
14 1 St to 7 th valves V1 to V7
The valve is made of common high-pressure valve, the pipe diameter at two ends is 6mm, stainless steel is adopted, and the pressure resistance is 50MPa.
2. Method for testing water retention parameter of tetrahydrofuran-containing hydrate soil (short method)
The method comprises the following steps:
① Sample preparation
According to the saturation degree of the target hydrate, preparing tetrahydrofuran water solutions with different concentrations, vacuumizing a sample 4-5, then saturating for 24 hours, opening 4 th to 7 th valves V4-V7, a refrigerating system 13 and a circulating pump 12, filling the saturated sample 4-5 into a sealing bag, placing the sealing bag into a water bath 10, cooling to-8 ℃ for induction, heating the water bath 10 to 1 ℃ after 3d, and keeping for 14d to enable THF to be completely converted into THF hydrate;
the preparation method of the tetrahydrofuran aqueous solution comprises the following steps:
m H2O -mass of water in the aqueous tetrahydrofuran solution;
m THF -mass of tetrahydrofuran in the aqueous solution of tetrahydrofuran;
S H, hydrate saturation;
② Sample loading
Considering the extra heat loss of the pressure chamber 4 in the heat transfer process, the water bath temperature should have a certain supercooling degree, and the temperature of the constant-temperature water bath 10 is reduced to minus 1 ℃; sealing the saturated clay plate 4-6 on the pressure chamber base 4-10 by using the 2 nd sealing rubber ring 4-7, opening the 1 st valve V1, and saturating the drainage groove 4-12 and the pipeline by water in the water storage bottle 5 through the water inlet 4-9; then, in order to ensure that the liquid collected in the liquid collecting cup 7 is discharged as the sample 4-5, the 2 nd valve V2 and the 3 rd valve V3 are opened, so that water passes through the pipeline and fills the gas collecting pipe 6, the gas in the gas collecting pipe 6 is discharged, and the 1 st valve V1 is closed; meanwhile, the liquid collecting cup 7 is sealed to prevent water loss; weighing a prefabricated saturated THF-containing hydrate sample 4-5, placing the sample on a clay plate 4-6, placing a1 st sealing rubber ring 4-2 into a notch of a pressure chamber upper cover 4-11, sealing the pressure chamber 4, and installing a fixing screw 4-3; the whole pressure chamber 4 is placed into a constant-temperature water bath 10, and after all pipelines are connected, the upper cover 4-11 of the water bath is closed;
③ Leak detection and pressurization
Peeling a balance 8 provided with a liquid collecting cup 7, opening a data acquisition system 9, opening an air valve of the high-pressure nitrogen cylinder 1, controlling a pressure reducing valve 2 and a pressure regulating pump 3 to introduce specified air pressure into a pressure chamber 4, filling an applied air pressure value in the data acquisition system 9, and setting a data acquisition time interval; if the pressure is unchanged after the first-stage pressure is applied for 2 hours, the tightness of the pressure chamber can be considered to be good, and the test can be continued;
④ Testing
After the pressure is applied, the water discharged by the samples 4-5 enters the liquid collecting cup 7 through a pipeline, and the data acquisition system 9 reads the reading of the balance 8 in real time to judge whether the suction force of the matrix reaches balance or not; after the balance 8 is stable in reading, the next stage of pressure can be applied;
⑤ Calculation of
And (3) according to the mass and water yield of saturated THF-containing hydrate samples 4-5 measured before the test, converting the water content of each stage after suction balance, and then establishing a soil-water characteristic relation curve (SWCC) of THF hydrate sediment according to the suction value and the water content of each stage.
Claims (2)
1. The utility model provides a contain tetrahydrofuran hydrate soil water retention parameter testing arrangement which characterized in that:
comprises a testing part and a water bath constant temperature part;
The test part comprises a high-pressure nitrogen bottle (1), a pressure reducing valve (2), a pressure regulating pump (3), a pressure chamber (4), a water storage bottle (5), a gas collecting tube (6), a liquid collecting cup (7), a balance (8), a data acquisition system (9) and 1 st to 3 rd valves (V1 to V3);
the water bath constant temperature part comprises a constant temperature water bath box (10), a temperature sensor (11), a circulating pump (12), a refrigerating system (13) and 4 th to 7 th valves (V4 to V7);
the positions and the connection relations are as follows:
A pressure chamber (4) is arranged in the constant-temperature water bath box (10), and a sample (4-5) and a clay plate (4-6) which are connected up and down are arranged in the pressure chamber (4) to provide a test place for the sample (4-5);
the high-pressure nitrogen cylinder (1), the pressure reducing valve (2) and the pressure regulating pump (3) are connected to an air inlet (4-1) of the pressure chamber upper cover (4-11) through pipelines in sequence to provide a pneumatic environment for the sample (4-5);
the water storage bottle (5), the 1 st valve (V1) and the water inlet (4-9) of the pressure chamber (4) are sequentially communicated to provide a hydraulic environment for the sample (4-5);
The water outlet (4-8) of the pressure chamber (4), the 2 nd valve (V2), the gas collecting pipe (6), the 3 rd valve (V3) and the liquid collecting cup (7) are sequentially communicated, the liquid collecting cup (7) is arranged on the balance (8), the balance (8) is connected with the data acquisition system (9), and the change of the water outlet of the sample (4-5) is measured;
the probes of the temperature sensor (11) are respectively arranged at the top, the middle and the bottom in the constant-temperature water bath box (10), the temperature sensor (11) is connected with the data acquisition system (9), and the temperature of the surrounding environment of the sample (4-5) is measured;
A heat conduction copper pipe (10-4) is arranged in the constant temperature water bath box (10), and a refrigerating fluid inlet (10-5), a water circulation inlet (10-6), a refrigerating fluid outlet (10-7) and a water circulation outlet (10-8) are respectively arranged on the left side wall and the right side wall of the constant temperature water bath box (10);
The water circulation inlet (10-6), the 5 th valve (V5), the circulation pump (12), the 6 th valve (V6) and the water circulation outlet (10-8) are sequentially communicated in a closed loop manner, so that a constant temperature environment is provided for the sample (4-5);
The outlet of the refrigerating system (13), the 4 th valve (V4), the refrigerating fluid inlet (10-5), the heat conduction copper pipe (10-4), the refrigerating fluid outlet (10-7), the 7 th valve (V7) and the inlet of the refrigerating system (13) are sequentially communicated in a closed loop manner, so that a refrigerating environment is provided for the sample (4-5);
The pressure chamber (4) comprises an air inlet (4-1), a1 st sealing rubber ring (4-2), a fixing screw (4-3), an organic glass cover (4-4), a sample (4-5), a clay plate (4-6), a2 nd sealing rubber ring (4-7), a water outlet (4-8), a water inlet (4-9), a pressure chamber base (4-10), an upper cover (4-11) and a drainage groove (4-12);
the positions and the connection relations are as follows:
the pressure chamber base (4-10), the organic glass cover (4-4) and the upper cover (4-11) are connected into a sealed container through 3 uniformly distributed fixing screws (4-3), and the joint is sealed by an O-shaped 1 st sealing rubber ring (4-2) and a2 nd sealing rubber ring (4-7);
an air inlet (4-1) is arranged on the upper cover (4-11);
The diameter phi of the clay plate (4-6) is 130mm, the 2 nd sealing rubber ring (4-7) is embedded at the top of the pressure chamber base (4-10), a sample (4-5) is arranged above the clay plate (4-6), and a drainage groove (4-12), a water outlet (4-8) and a water inlet (4-9) are arranged below the clay plate (4-6);
The constant-temperature water bath box (10) comprises a water bath box upper cover (10-1), an upper cover handle (10-2), a water bath box body (10-3), a heat conduction copper pipe (10-4), a refrigerating fluid inlet (10-5), a water circulation inlet (10-6), a refrigerating fluid outlet (10-7) and a water circulation outlet (10-8);
the positions and the connection relations are as follows:
The upper cover (10-1) of the water bath box and the water bath box body (10-3) are connected up and down to form a whole;
an upper cover handle (10-2) is arranged on the upper cover (10-1) of the water bath box;
The upper part and the lower part in the water bath box body (10-3) are respectively provided with a heat conduction copper pipe (10-4);
The upper part of the inner wall of the water bath box body (10-3) is respectively provided with a refrigerating fluid inlet (10-5) and a water circulation inlet (10-6);
a refrigerating fluid outlet (10-7) and a water circulation outlet (10-8) are respectively arranged at the lower part of the inner wall of the water bath box body (10-3);
The upper cover (10-1) of the water bath box is formed by combining two small rectangular covers with connecting openings, the size is 40cm multiplied by 40cm, the thickness is 3cm, and the inside is filled with heat preservation and insulation materials; the opening size diameter d=4 cm;
The water bath box body (10-3) is a square container with the size of 40cm multiplied by 50cm and the thickness of 3cm, and the inside is filled with heat preservation and insulation materials.
2. A testing method based on the testing device according to claim 1, characterized in that:
The method comprises the following steps:
① Sample preparation
According to the saturation degree of the target hydrate, tetrahydrofuran water solutions with different concentrations are prepared, the sample (4-5) is vacuumized and then saturated for 24 hours, the 4 th to 7 th valves (V4 to V7), the refrigerating system (13) and the circulating pump (12) are opened, the saturated sample (4-5) is put into a sealing bag and placed into a constant-temperature water bath (10) to be cooled to-8 ℃ for induction, and after 3d, the constant-temperature water bath (10) is heated to 1 ℃ and kept for 14d, so that THF is completely converted into THF hydrate;
the preparation method of the tetrahydrofuran aqueous solution comprises the following steps:
-the mass of water in the aqueous tetrahydrofuran solution;
-the mass of tetrahydrofuran in the aqueous solution of tetrahydrofuran;
-hydrate saturation;
② Sample loading
Considering the extra heat loss of the pressure chamber (4) in the heat transfer process, the water bath temperature should have a certain supercooling degree, and the temperature of the constant-temperature water bath box (10) is reduced to minus 1 ℃; sealing the saturated clay plate (4-6) on a pressure chamber base (4-10) by a2 nd sealing rubber ring (4-7), opening a1 st valve (V1), and saturating the drainage groove (4-12) and the pipeline by water in the water storage bottle (5) through a water inlet (4-9); then, in order to ensure that the liquid collected in the liquid collecting cup (7) is discharged as a sample (4-5), a2 nd valve (V2) and a 3 rd valve (V3) are opened, water is enabled to pass through a pipeline and fill the gas collecting pipe (6), gas in the gas collecting pipe (6) is discharged, and a1 st valve (V1) is closed; meanwhile, the liquid collecting cup (7) should be sealed to prevent water loss; weighing a prefabricated saturated THF-containing hydrate sample (4-5), placing the sample on a clay plate (4-6), placing a1 st sealing rubber ring (4-2) into a notch of a pressure chamber upper cover (4-11), sealing the pressure chamber (4), and installing a fixing screw (4-3); the whole pressure chamber (4) is placed into a constant-temperature water bath box (10), and after all pipelines are connected, the upper cover (4-1) of the water bath box is closed;
③ Leak detection and pressurization
Peeling a balance (8) provided with a liquid collecting cup (7), opening a data acquisition system (9), opening an air valve of a high-pressure nitrogen cylinder (1), controlling a pressure reducing valve (2) and a pressure regulating pump (3) to introduce specified air pressure into a pressure chamber (4), filling an applied air pressure value in the data acquisition system (9), and setting a data acquisition time interval; if the pressure is unchanged after the first-stage pressure is applied for 2 hours, the tightness of the pressure chamber can be considered to be good, and the test can be continued;
④ Testing
After the pressure is applied, the water discharged by the sample (4-5) enters the liquid collecting cup (7) through the pipe, and the data acquisition system (9) reads the reading of the balance (8) in real time to judge whether the suction of the matrix reaches the balance or not; after the reading of the balance (8) is stable, the next stage of pressure can be applied;
⑤ Calculation of
And (3) according to the mass and water yield of saturated THF-containing hydrate samples (4-5) measured before the test, converting the water content of each stage after suction balance, and then establishing a soil-water characteristic relation curve of THF hydrate sediment according to the suction value and the water content of each stage.
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