CN109991114A - The retentiveness parameter test device of soil containing Tetrahydrofuran hydrate and its method - Google Patents
The retentiveness parameter test device of soil containing Tetrahydrofuran hydrate and its method Download PDFInfo
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- CN109991114A CN109991114A CN201910184328.6A CN201910184328A CN109991114A CN 109991114 A CN109991114 A CN 109991114A CN 201910184328 A CN201910184328 A CN 201910184328A CN 109991114 A CN109991114 A CN 109991114A
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- 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
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- 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
Abstract
The invention discloses a kind of retentiveness parameter test device of soil containing Tetrahydrofuran hydrate and its methods, are related to a kind of measuring technology of the retentiveness of soil containing hydrate parameter.The present apparatus includes part of detecting and constant temperature water bath part；Part of detecting includes high-pressure nitrogen bottle (1), pressure reducing valve (2), pressure adjusting pump (3), pressure (4), water-storing bottle (5), gas collecting tube (6), liquid collecting cup (7), balance (8), data collection system (9) and the 1st~3 valve (V1~V3)；Constant temperature water bath part includes constant water bath box (10), circulating pump (11), temperature sensor (12), refrigeration system (13) and the 4th~7 valve (V4~V7).Simple and quick uniform and stable soil sample containing hydrate can be made in the present invention；Easy it can quick and precisely obtain SWCC curve；Suction force range is wider, can be reduced the human error of traditional whole translation method test.
Description
Technical field
The present invention relates to a kind of measuring technologies of the retentiveness of soil containing hydrate parameter, more particularly to one kind to contain tetrahydrofuran
(THF) hydrate soil retentiveness parameter test device and its method.
Specifically, under the conditions of being related to different hemihydrate contents the soil containing Tetrahydrofuran hydrate native water characteristic relation curve
(SWCC) it measures, sample control is formed into Tetrahydrofuran hydrate under cryogenic and tests, utilize axial translation technology
The control and measurement for carrying out suction, are acquired record to sample water yield according to automatic data acquisition system, judge that suction is flat
The water content of weighing apparatus and calculating sample under the suction obtains the soil under the conditions of the different hemihydrate contents of the soil containing Tetrahydrofuran hydrate
Water characteristic relation curve provides significant data for hydrate exploitation and supports.
Background technique
Gas hydrates are a kind of novel clean energy, however exploit and improper will lead to submarine landslide, surface collapse etc.
Engineering problem, can also release greenhouse gases leads to global warming.Water retention characteristic parameter containing hydrate sediment is day
Very important underlying parameter in right gas hydrate probing and recovery process, the mechanical property of deposit, are assigned air water transition process
It is all related with its water retention property to deposit state.Native water characteristic relation curve (SWCC) is that the relationship between water content of soil and suction is bent
Line reflects the moisture holding capacity of the soil body, is the Key Functions for describing unsaturated soil behavior.SWCC curve is substantially by hole ruler
Spend what feature determined, including pore shape and size distribution, interconnectivity and space variance, fluid and interfacial tension etc., deposition
The hydrate of preservation can largely change the pore scale feature of the soil body in object.
The research for carrying out the curve of SWCC containing hydrate sediment has very big difficulty, and the decomposition of hydrate is avoided to need height
Fluid pressure and cryogenic conditions；Synthesizing methane hydrate needs longer induction time in the lab simultaneously, and methane is in water
Solubility is low, infiltration loss is big, it is difficult to keep sample to stablize in test, and synthesis is expensive with testing equipment, so that related
Data are extremely deficient.Studies have shown that tetrahydrofuran (THF) hydrate and methane hydrate have similar thermophysical property, it can
Overcome above difficult and substitute methane hydrate progress experimental study, synthesizes and only need to control cryogenic conditions, and THF hydrate
Saturation degree is easily controllable, therefore we use THF hydrate as subjects, has developed for testing THF hydrate deposition
The laboratory testing rig of object SWCC curve.The device can overcome common pressure plare method in native water characteristic relation curve test
Time-consuming, suction force range is small, test data need it is periodically artificial read cause error, without temperature-controlling system the disadvantages of, can be not only used for THF
The test of hydrate sediment SWCC curve, it can also be used to the test of conventional examples.
Currently, studying and being had not been reported with the device and method of the test retentiveness of soil containing hydrate parameter through retrieving.
Summary of the invention:
It is an object of the invention to fill up obtaining the parameter of retentiveness containing hydrate sediment laboratory testing rig both at home and abroad
On blank, overcome the deficiencies in the prior art described above, a kind of retentiveness parameter testing of soil containing Tetrahydrofuran hydrate be provided and is filled
Set and its method, design rationally, it is easy to be easy-to-use, the measurement result of the native water characteristic relation curve of THF hydrate can be made accurate,
Test is time-consuming short, and measuring method is convenient.
The present invention in order to solve the above problem the technical solution adopted is that:
The present apparatus is to apply air pressure to the sample in pressure chamber using nitrogen under cryogenic, is controlled using whole translation method
With measure the sample of hydrate containing THF suction, acquisition according to automatic data acquisition system to sample water yield judges suction equalization
With water content of the calculating sample under the suction, the soil-water characteristic curve (SWCC) of the soil containing Tetrahydrofuran hydrate is obtained, big
The retentiveness parameter study of the warp containing hydrate is realized while shortening test period greatly, principle meets hydrate shape
At mode and exploitation working condition, structure is simple, cheap, can equip for most of scientific researches and designing unit.
This method is that after being placed in a certain concentration aqueous tetrahydrofuran solution and being saturated by sample, which is placed in constant temperature
Cool down induction in water-bath, and obtained hydrate is evenly distributed native containing Tetrahydrofuran hydrate；It will contain at THF hydrate sample loading
On pottery clay plates in the pressure chamber of water bath with thermostatic control, air pressures at different levels are applied to pressure chamber, are contained using whole translation method control and measurement
THF hydrate sample suction, data collection system automatic collection records the water yield data of sample in pressure chamber, according to water yield
State can quickly judge sample balance and water content, obtain the native water characteristic relation curve under the conditions of different hydrate concentrations
(SWCC), method is simply accurate, easily operated.
Specifically:
One, the retentiveness of soil containing Tetrahydrofuran hydrate parameter test device
The present apparatus includes part of detecting and constant temperature water bath part；
Part of detecting include high-pressure nitrogen bottle, pressure reducing valve, pressure adjust pump, pressure chamber, water-storing bottle, gas collecting tube, liquid collecting cup,
Balance, data collection system and the 1st~3 valve；
Constant temperature water bath part includes constant water bath box, temperature sensor, circulating pump, refrigeration system and the 4th~7 valve；
Its position and connection relationship are:
It is provided with pressure chamber in constant water bath box, the sample and pottery clay plates being vertically connected with are provided in pressure chamber, is given
Sample provides the place of test；
High-pressure nitrogen bottle, pressure reducing valve and pressure adjust the air inlet that pump passes sequentially through piping connection to pressure chamber upper cover, give
Sample provides air pressure environment；
The water inlet of water-storing bottle, the 1st valve and pressure chamber is sequentially communicated, and provides hydraulic pressure environment to sample；
The water outlet of pressure chamber, the 2nd valve, gas collecting tube, the 3rd valve and liquid collecting cup are sequentially communicated, and liquid collecting cup is placed in balance
On, balance is connected with data collection system, the variation of measurement sample water outlet；
The probe of temperature sensor is set to top, centre, bottom in constant water bath box, and temperature sensor and data are adopted
Collecting system connects, and measures the temperature of sample ambient enviroment；
Heat-conducting copper pipe is provided in constant water bath box, the left and right sidewall of constant water bath box be respectively arranged with refrigerating fluid into
Mouth, the import of water circulation, refrigerating fluid outlet and water loop exit；
The import of water circulation, the 5th valve V5 circulating pump, successively closed loop is connected to the 6th valve with water loop exit, and sample is given to provide
Isoperibol；
The outlet of refrigeration system, the 4th valve, refrigerating fluid import, heat-conducting copper pipe, refrigerating fluid outlet, the 7th valve and refrigeration system
Successively closed loop is connected to the entrance of system, provides refrigerating environment to sample.
Working principle:
The present apparatus carries out temperature control using constant temperature water bath system, to a certain concentration tetrahydrofuran solution in constant temperature water bath system
The sample of saturation carries out cooling induction, and the sample of hydrate containing THF that different hemihydrate contents are quickly made and are evenly distributed will contain
After THF hydrate sample is placed on the indoor pottery clay plates of pressure, pressure chamber's assembling is finished and is placed in constant water bath box, height is used
Nitrogen cylinder is pressed to apply air pressures at different levels to pressure chamber, it is defeated to pressure chamber that nitrogen cylinder mesohigh gas can be become low-pressure gas by pressure reducing valve
It send, pressure adjusting pump can be pressurized or release, and for adjusting air pressure in pressure chamber, water-storing bottle is for carrying out at saturation whole system
Reason, and make water full of entire test pipeline, gas collecting tube is for the gas in test adjustment stage collecting to ensure liquid collecting
The liquid collected in cup is really sample discharge, and liquid collecting cup is used to collect the moisture of sample discharge, and biodiversity is by being connected to data
The balance of acquisition system carries out automatic reading and record, can quickly judge sample balance and water content according to water yield state, obtain
Native water characteristic relation curve (SWCC) under the conditions of different hydrate concentrations out.
The present invention has the advantages that:
1, simple and quick uniform and stable soil sample containing hydrate can be made；
2, easy SWCC curve can quick and precisely be obtained；
3, suction force range is wider, can be reduced the human error of traditional whole translation method test.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the present apparatus；
Fig. 2 is the structural schematic diagram of pressure chamber；
Fig. 3 is the structural schematic diagram of constant water bath box.
Wherein:
1-high-pressure nitrogen bottle；
2-pressure reducing valves；
3-pressure adjust pump；
4-pressure chambers,
The 1st sealing rubber ring of 4-1-air inlet, 4-2-, 4-3-standing screw,
4-4-organic glass, 4-5-sample, 4-6-pottery clay plates,
The 2nd sealing rubber ring of 4-7-, 4-8-water outlet, 4-9-water inlet,
4-10-pressure chamber base, 4-11-pressure chamber upper cover, 4-12-drainage groove；
5-water-storing bottles；
6-gas collecting tubes；
7-liquid collecting cups；
8-balances；
9-data collection systems；
10-constant water bath box,
10-1-water-bath box cover, 10-2-upper cover handle, 10-3-water-bath cabinet,
10-4-heat-conducting copper pipe, 10-5-refrigerating fluid import, 10-6-water recycle import,
10-7-refrigerating fluid outlet, 10-8-water loop exit；
11-temperature sensors；
12-circulating pumps；
13-refrigeration systems；
V1, V2 ,~V7-the 1st, 2~7 valves.
Specific embodiment
One, device
1, overall
Such as Fig. 1,2,3, the present apparatus includes part of detecting and constant temperature water bath part；
Part of detecting include high-pressure nitrogen bottle 1, pressure reducing valve 2, pressure adjust pump 3, pressure chamber 4, water-storing bottle 5, gas collecting tube 6,
Liquid collecting cup 7, balance 8, data collection system 9 and the 1st~3 valve V1~V3；
Constant temperature water bath part includes constant water bath box 10, temperature sensor 11, circulating pump 12, refrigeration system 13 and the 4th~7
Valve V4~V7；
1) part of detecting
High-pressure nitrogen bottle 1, pressure reducing valve 2 and pressure adjust pump 3 pass sequentially through piping connection to pressure chamber upper cover 4-11 into
Port 4-1 the case where in order to preferably observe sample 4-5, uses plexiglass tent 4-4 to pass through three as the outer wall of pressure chamber 4
Pressure chamber upper cover 4-11, plexiglass tent 4-4 are connect by a standing screw 4-3 with pressure chamber base 4-10, plexiglass tent 4-4
Upper limb and pressure chamber upper cover 4-11 are sealed by the 1st sealing rubber ring 4-2, pass through the 2nd sealing rubber ring 4-7 with pressure chamber base 4-10
Sealing, while the 2nd sealing rubber ring 4-7 also seals fixed pottery clay plates 4-6, sample 4-5 is placed on pottery clay plates 4-6, pottery clay plates 4-6
Lower section is equipped with drainage groove 4-12, water outlet 4-8 and water inlet 4-9, and water inlet 4-9 is connected to by pipeline and the 1st valve V1
Water-storing bottle 5, water outlet 4-8 are connected to gas collecting tube 6 by pipeline and the 2nd valve V2, and gas collecting tube 6 passes through pipeline and the 3rd valve V3
It is connected in liquid collecting cup 7, liquid collecting cup 7 is placed on balance 8, and balance 8 is connected to data collection system 9, and data collection system 9 passes through
It is automatic to read 8 read-record sample water yield of balance, and water yield and time curve are drawn automatically.
2) constant temperature water bath part
THF gas hydrate synthesis needs low temperature environment, therefore the pressure for the sample of hydrate containing THF 4-5 being placed in part of detecting
Power room 4 is placed in constant water bath box 10 and is tested, and refrigerating fluid is configured by ethylene glycol and distilled water by 1:2；Water bath with thermostatic control
Case 10 is made of cabinet 10-3 and upper cover 10-1 two parts, and upper cover 10-1 is that two small rectangles are closed with the lid of connection aperture
And form, convenient for the piping connection of pressure chamber 4, heat-conducting copper pipe 10-4 is equipped in cabinet 10-3 and carries out refrigerating fluid circulation, by freezing
System 13 cools down to refrigerating fluid, and refrigerating fluid is by refrigeration system 13 by way of pipeline and the 4th valve V4 from refrigerating fluid import 10-5
Refrigeration system 13 is returned to by way of pipeline and the 7th valve V7 into heat-conducting copper pipe 10-4, and by refrigerating fluid outlet 10-7；To guarantee
Bath temperature is uniform in cabinet 10-3, and circulating pump 12 is arranged outside water bath 10 and carries out water circulation, water is by water loop exit in cabinet
10-8 enters water circulation import 10-6 by way of pipeline, the 6th valve V6, circulating pump 12 and the 5th valve V5；In order to detect water bath 10
Whether temperature reaches target temperature and temperature is uniform, and 3 in temperature sensor 11 temp probe is separately positioned in water bath
10 top, centre, bottom, and by data automatic recording in data collection system 9.
Its position and connection relationship are:
It is provided with pressure chamber 4 in constant water bath box 10, the sample 4-5 and pottery being vertically connected with are provided in pressure chamber 4
Native plate 4-6 provides the place of test to sample 4-5；
High-pressure nitrogen bottle 1, pressure reducing valve 2 and pressure adjust pump 3 pass sequentially through piping connection to pressure chamber upper cover 4-11 into
Port 4-1 provides air pressure environment to sample 4-5；
The water inlet 4-9 of water-storing bottle 5, the 1st valve V1 and pressure chamber 4 is sequentially communicated, and provides hydraulic pressure environment to sample 4-5；
Water outlet 4-8, the 2nd valve V2, gas collecting tube 6, the 3rd valve V3 and the liquid collecting cup 7 of pressure chamber 4 are sequentially communicated, liquid collecting
Cup 7 is placed on balance 8, and balance 8 and data collection system 9 connect, the variation of measurement sample 4-5 water outlet；
The probe of temperature sensor 11 is respectively arranged at top, centre, bottom in constant water bath box 10, temperature sensor
11 and data collection system 9 connect, measure sample 4-5 ambient enviroment temperature；
It is provided with heat-conducting copper pipe 10-4 in constant water bath box 10, is respectively arranged in the left and right sidewall of constant water bath box 10
Refrigerating fluid import 10-5, water circulation import 10-6, refrigerating fluid export 10-7 and water loop exit 10-8；
Water recycles import 10-6, the 5th valve V5, circulating pump 12, the 6th valve V6 and water loop exit 10-8, and successively closed loop connects
It is logical, isoperibol is provided to sample 4-5；
The outlet of refrigeration system 13, the 4th valve V4, refrigerating fluid import 10-5, heat-conducting copper pipe 10-4, refrigerating fluid export 10-
7, successively closed loop is connected to the 7th valve V4 with the entrance of refrigeration system 13, provides refrigerating environment to sample 4-5.
2, functional component
1) high-pressure nitrogen bottle 1
It is a kind of ordinary nitrogen storage cylinder, is provided by Guangdong South China Special Gas Institute Co., Ltd..
2) pressure reducing valve 2
Select Shanghai Wei Yue Industrial Co., Ltd. product, model: YQY-12, input pressure 15Mpa, adjustable range 0.1-
1.25MPa。
3) pressure adjusts pump 3
Select Fairchild Industrial Products Company product, model: M30BP, adjustable range: 0-
15kPa, 15-700kPa, maximum pressure: 1000kpa, precision: 0.15psi.
4) pressure chamber 4
Such as Fig. 2, pressure chamber 4 include air inlet 4-1, the 1st sealing rubber ring 4-2, standing screw 4-3, plexiglass tent 4-4,
Sample 4-5, pottery clay plates 4-6, the 2nd sealing rubber ring 4-7, water outlet 4-8, water inlet 4-9, pressure chamber base 4-10, upper cover 4-11
Number drainage groove 4-12；
Its position and connection relationship are:
From top to bottom, pedestal 4-10, plexiglass tent 4-4 and upper cover 4-11 are connected by 3 uniformly distributed standing screw 4-3
At a sealing container, interface is sealed processing by O-shaped 1st sealing rubber ring 4-2 and the 2nd sealing rubber ring 4-7；
Air inlet 4-1 is provided on upper cover 4-11；
Pottery clay plates 4-6 diameterBy the 2nd sealing rubber ring 4-7 at the top of pedestal 4-10, in the upper of pottery clay plates 4-6
Side is provided with sample 4-5, and drainage groove 4-12, water outlet 4-8 and water inlet 4-9 are provided with below pottery clay plates 4-6.
5) water-storing bottle 5
It is a kind of common water-storing bottle, capacity 2L.
6) gas collecting tube 6
It is a kind of common gas collecting tube with a scale, capacity 15ml, precision 0.5ml.
7) liquid collecting cup 7
It is a kind of common beaker, capacity 200ml does encapsulation process, and rim of a cup reserves an aperture connecting line.
8) balance 8
Using Ohaus brand electronic scale, model: Scout pro SP202 is weighed: 200g, precision: 0.01g.
9) data collection system 9
Agilent data collecting instrument and data acquisition software are selected, model: 34972A, the channel provided by collector
Connection balance 8 and temperature sensor 11 are acquired data and record, handle.
10) constant water bath box 10
Such as Fig. 3, constant water bath box 10 includes water-bath box cover 10-1, upper cover handle 10-2, water-bath cabinet 10-3, conduction copper
Pipe 10-4, refrigerating fluid import 10-5, water circulation import 10-6, refrigerating fluid export 10-7, water loop exit 10-8；
Its position and connection relationship are:
Water-bath box cover 10-1 and water-bath cabinet 10-3 are vertically connected with into an entirety；
Upper cover handle 10-2 is provided on water-bath box cover 10-1；
Upper and lower part in water-bath cabinet 10-3 is provided with heat-conducting copper pipe 10-4 respectively；
Refrigerating fluid import 10-5, water circulation import 10-6 are respectively arranged on the top of water-bath cabinet 10-3 inner wall；
Refrigerating fluid outlet 10-7 and water loop exit 10-8 is respectively arranged in the lower part of water-bath cabinet 10-3 inner wall.
(1) water-bath box cover 10-1
Merge for two small rectangles with the lid of connection aperture, having a size of 40cm × 40cm, thick 3cm is internal
Fill heat preserving and insulating material；Aperture size diameter d=4cm.
(2) upper cover handle 10-2
Common part.
(3) water-bath cabinet 10-3
Square container, having a size of 40cm × 40cm × 50cm, thick 3cm, inside filling heat preserving and insulating material.
Four drillings: refrigerating fluid import 10-5, water circulation import 10-6, refrigerating fluid outlet 10-7, water loop exit are set
10-8, diameter d=1cm, the wall of a borehole do encapsulation process.
(4) heat-conducting copper pipe 10-4
It is folded to be close to cabinet 10-3 internal helicoid formula disk by common part, 1/2 pipe, outer diameter 12.7mm.
11) circulating pump 11
Jiangsu Sheng Lan instrument manufacturing Co., Ltd product is selected, model: BT-200B, binary channels output, output flow: 2 ×
(1~6800) ml/h, output pressure: >=2.5kg/cm2.
12) temperature sensor 12
Totally 3, Beijing match hundred million is selected to insult Science and Technology Ltd.'s product, name of product: pt100, model: 1632-100, work
Make temperature: -40~450 DEG C, error: ± (0.15+0.002 ∣ t ∣).
13) refrigeration system 13
Ningbo Tian Heng instrument plant low temperature thermostat bath product is selected, model: THD-2030, temperature range:
- 20 DEG C~100 DEG C, control precision: 0.01 DEG C, built-in circulating pump, pump discharge 13L/min.
14) the 1st~7 valve V1~V7
Using ordinary high pressure valve, both ends caliber Φ 6mm is made, pressure-resistant 50MPa of stainless steel.
Two, the retentiveness of soil containing Tetrahydrofuran hydrate parameter test method (abbreviation method)
This method the following steps are included:
1. sample preparation
According to target hydrate concentration, the aqueous tetrahydrofuran solution of various concentration is configured, sample 4-5 is vacuumized laggard
Row saturation for 24 hours, opens the 4th~7 valve V4~V7, refrigeration system 13 and circulating pump 12, and the sample 4-5 after saturation is packed into sealing
Bag, which is placed in, to be cooled to -8 DEG C in water bath 10 and is induced, and water bath 10 is warming up to 1 DEG C of holding 14d after 3d, turns THF completely
Turn to THF hydrate；
Aqueous tetrahydrofuran solution configuration method are as follows:
mH2O--- the quality of water in aqueous tetrahydrofuran solution；
mTHF--- the quality of tetrahydrofuran in aqueous tetrahydrofuran solution；
SH--- hydrate concentration；
2. filling sample
In view of additional heat loss of the pressure chamber 4 in diabatic process, bath temperature should have certain degree of supercooling, reduce
The temperature of constant water bath box 10 is to -1 DEG C；The pottery clay plates 4-6 after saturation is sealed in pressure chamber base with the 2nd sealing rubber ring 4-7
4-10, opens the 1st valve V1, and the water in water-storing bottle 5 carries out at saturation drainage groove 4-12 and pipeline by water inlet 4-9
Reason；Then it is sample 4-5 discharge to make the liquid collected in liquid collecting cup 7 really, opens the 2nd valve V2 and the 3rd valve V3, keep water logical
It crosses pipeline and is full of gas collecting tube 6, gas in gas collecting tube 6 is discharged, closes the 1st valve V1；Also reply liquid collecting cup 7 is sealed simultaneously
Processing prevents moisture loss；Then the prefabricated saturation sample of hydrate containing THF 4-5 is weighed, is subsequently placed at pottery clay plates
On 4-6, by sealed pressure room 4 after the 1st sealing rubber ring 4-2 merging pressure chamber upper cover 4-11 notch and standing screw 4-3 is installed；It will
In the whole merging constant water bath box 10 in pressure chamber 4, by all piping connections it is good after close water-bath box cover 4-11；
3. leak detection and pressurization
The balance 8 for being placed with liquid collecting cup 7 is removed the peel, data collection system 9 is opened, opens the air valve of high-pressure nitrogen bottle 1, control
Pressure reducing valve 2 and pressure adjust pump 3 and are passed through specified air pressure into pressure chamber 4, fill in data collection system 9 and apply air pressure numerical value,
And data collection interval is set；After applying the first stage pressure 2h pressure show it is constant if it is believed that pressure chamber's leakproofness it is good
Good, test can proceed with；
4. testing
After applying pressure, the moisture of sample 4-5 discharge enters by the road in liquid collecting cup 7, and data collection system 9 is read in real time
Balance 8 is read to judge whether matric suction reaches balance；After 8 stable reading of balance, next stage pressure can be applied；
5. calculating
Suction equalizations at different levels are conversed according to saturation hydrate containing the THF sample 4-5 mass and water yield that measure before test
Moisture content afterwards, suction value and moisture content further according to every level-one establish the native water characteristic relation curve of THF hydrate sediment
(SWCC)。
Claims (4)
1. a kind of retentiveness parameter test device of soil containing Tetrahydrofuran hydrate, it is characterised in that:
Including part of detecting and constant temperature water bath part；
Part of detecting includes high-pressure nitrogen bottle (1), pressure reducing valve (2), pressure adjusting pump (3), pressure chamber (4), water-storing bottle (5), collection
Tracheae (6), liquid collecting cup (7), balance (8), data collection system (9) and the 1st~3 valve (V1~V3)；
Constant temperature water bath part includes constant water bath box (10), temperature sensor (11), circulating pump (12), refrigeration system (13) and
4~7 valves (V4~V7)；
Its position and connection relationship are:
It is provided with pressure chamber (4) in constant water bath box (10), the sample (4-5) being vertically connected with is provided in pressure chamber (4)
With pottery clay plates (4-6), the place of test is provided to sample (4-5)；
High-pressure nitrogen bottle (1), pressure reducing valve (2) and pressure adjust pump (3) and pass sequentially through piping connection to pressure chamber upper cover (4-11)
Air inlet (4-1), to sample 4-5 provide air pressure environment；
The water inlet (4-9) of water-storing bottle (5), the 1st valve (V1) and pressure chamber (4) is sequentially communicated, and provides hydraulic pressure to sample (4-5)
Environment；
Water outlet (4-8), the 2nd valve (V2), gas collecting tube (6), the 3rd valve (V3) and the liquid collecting cup (7) of pressure chamber (4) successively connect
Logical, liquid collecting cup (7) is placed on balance (8), balance (8) and data collection system (9) connection, the change of measurement sample (4-5) water outlet
Change；
The probe of temperature sensor (11) is respectively arranged at top, centre, bottom in constant water bath box (10), temperature sensor
(11) it is connected with data collection system (9), measures the temperature of sample (4-5) ambient enviroment；
It is provided with heat-conducting copper pipe (10-4) in constant water bath box (10), is respectively set in the left and right sidewall of constant water bath box (10)
There are refrigerating fluid import (10-5), water circulation import (10-6), refrigerating fluid outlet (10-7) and water loop exit (10-8)；
Water circulation import (10-6), the 5th valve (V5), circulating pump (12), the 6th valve (V6) and water loop exit (10-8) are successively
Closed loop connection provides isoperibol to sample (4-5)；
The outlet of refrigeration system (13), the 4th valve (V4), refrigerating fluid import (10-5), heat-conducting copper pipe (10-4), refrigerating fluid outlet
Successively closed loop is connected to the entrance of refrigeration system (13) for (10-7), the 7th valve (V4), provides refrigerating environment to sample (4-5).
2. the retentiveness of soil containing Tetrahydrofuran hydrate parameter test device according to claim 1, it is characterised in that:
The pressure chamber (4) includes air inlet (4-1), the 1st sealing rubber ring (4-2), standing screw (4-3), plexiglass tent
(4-4), sample (4-5), pottery clay plates (4-6), the 2nd sealing rubber ring (4-7), water outlet (4-8), water inlet (4-9), pressure chamber bottom
Seat (4-10), upper cover (4-11), drainage groove (4-12)；
Its position and connection relationship are:
From top to bottom, pedestal (4-10), plexiglass tent (4-4) and upper cover (4-11) pass through 3 uniformly distributed standing screws (4-3)
A sealing container is connected into, interface is sealed by the 1st O-shaped sealing rubber ring (4-2) and the 2nd sealing rubber ring (4-7)
Reason；
Air inlet (4-1) is provided on upper cover (4-11)；
Pottery clay plates (4-6) diameterBy the 2nd sealing rubber ring (4-7) at the top of pedestal (4-10), at pottery clay plates (4-6)
Top be provided with sample (4-5), be provided with below pottery clay plates (4-6) drainage groove (4-12), water outlet (4-8) and into
The mouth of a river (4-9).
3. the retentiveness of soil containing Tetrahydrofuran hydrate parameter test device according to claim 1, it is characterised in that:
The constant water bath box (10) includes water-bath box cover (10-1), upper cover handle (10-2), water-bath cabinet (10-3), is led
Hot copper pipe (10-4), refrigerating fluid import (10-5), water circulation import (10-6), refrigerating fluid outlet (10-7) and water loop exit
(10-8)；
Its position and connection relationship are:
Water-bath box cover (10-1) and water-bath cabinet (10-3) are vertically connected with into an entirety；
Upper cover handle (10-2) is provided on water-bath box cover (10-1)；
Upper and lower part in water-bath cabinet (10-3) is provided with heat-conducting copper pipe (10-4) respectively；
Refrigerating fluid import (10-5), water circulation import (10-6) are respectively arranged on the top of water-bath cabinet (10-3) inner wall；
Refrigerating fluid outlet (10-7) and water loop exit (10-8) are respectively arranged in the lower part of water-bath cabinet (10-3) inner wall；
Water-bath box cover (10-1) is that two small rectangles merge with the lid of connection aperture, having a size of 40cm ×
40cm, thick 3cm, inside filling heat preserving and insulating material；Aperture size diameter d=4cm；
Water-bath cabinet (10-3) is square container, having a size of 40cm × 40cm × 50cm, thick 3cm, and inside filling insulation material
Material.
4. the test method based on test device described in claim 1-3, it is characterised in that:
This method the following steps are included:
1. sample preparation
According to target hydrate concentration, the aqueous tetrahydrofuran solution of various concentration is configured, is carried out after being vacuumized to sample (4-5)
Saturation for 24 hours, opens the 4th~7 valve (V4~V7), refrigeration system (13) and circulating pump (12), and the sample (4-5) after saturation is filled
Enter hermetic bag and be placed in be cooled to -8 DEG C in water bath (10) and induced, water bath (10) is warming up to 1 DEG C of holding 14d after 3d,
THF is set to be fully converted to THF hydrate；
Aqueous tetrahydrofuran solution configuration method are as follows:
mH2O--- the quality of water in aqueous tetrahydrofuran solution；
mTHF--- the quality of tetrahydrofuran in aqueous tetrahydrofuran solution；
SH--- hydrate concentration；
2. filling sample
In view of the additional heat loss of pressure chamber (4) in diabatic process, bath temperature should have certain degree of supercooling, reduce permanent
The temperature of warm water bath cabinet (10) is to -1 DEG C；The pottery clay plates (4-6) after saturation are sealed in pressure chamber with the 2nd sealing rubber ring (4-7)
Pedestal (4-10) opens the 1st valve (V1), and the water in water-storing bottle (5) is by water inlet (4-9) to drainage groove (4-12) and pipe
Road carries out saturated process；Then to make the liquid collected in liquid collecting cup (7) really be sample (4-5) discharge, the 2nd valve (V2) is opened
It with the 3rd valve (V3), passes water through pipeline and is full of gas collecting tube (6), gas in discharge gas collecting tube (6) closes the 1st valve
(V1)；Also reply liquid collecting cup (7) is sealed processing and prevents moisture loss simultaneously；Then prefabricated saturation is hydrated containing THF
Object sample (4-5) is weighed, and is subsequently placed on pottery clay plates (4-6), and the 1st sealing rubber ring (4-2) is placed in pressure chamber upper cover (4-
11) sealed pressure room (4) and standing screw (4-3) is installed after notch；By pressure chamber (4) integrally merging constant water bath box (10)
In, by all piping connections it is good after close water-bath box cover (4-11)；
3. leak detection and pressurization
The balance (8) for being placed with liquid collecting cup (7) is removed the peel, data collection system () 9 is opened, opens the air valve of high-pressure nitrogen bottle (1),
Control pressure reducing valve (2) and pressure adjust pump (3) and are passed through specified air pressure in pressure chamber (4), fill in and apply in data collection system (9)
Numerical value with air pressure capable of being increased, and data collection interval is set；After applying the first stage pressure 2h pressure show it is constant if it is believed that pressure
Power room leakproofness is good, and test can proceed with；
4. testing
After applying pressure, the moisture of sample (4-5) discharge enters by the road in liquid collecting cup (7), and data collection system (9) is read in real time
Take balance (8) reading to judge whether matric suction reaches balance；After balance (8) stable reading, next stage pressure can be applied
Power；
5. calculating
After conversing suction equalizations at different levels according to the saturation sample of hydrate containing THF (4-5) quality and water yield that measure before test
Moisture content, suction value and moisture content further according to every level-one establish the native water characteristic relation curve of THF hydrate sediment.
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| CN201910184328.6A CN109991114A (en) | 2019-03-12 | 2019-03-12 | The retentiveness parameter test device of soil containing Tetrahydrofuran hydrate and its method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111965017A (en) * | 2020-07-15 | 2020-11-20 | 中国地质大学（武汉） | Method for measuring tensile strength of hydrate deposit |
| CN114965142A (en) * | 2022-08-02 | 2022-08-30 | 中国科学院地质与地球物理研究所 | Device for testing soil-water characteristic curve of hydrate deposit |
| CN115165652A (en) * | 2022-07-27 | 2022-10-11 | 中国科学院武汉岩土力学研究所 | Testing device for suction force of sludge soil matrix and implementation method thereof |
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2019
- 2019-03-12 CN CN201910184328.6A patent/CN109991114A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111965017A (en) * | 2020-07-15 | 2020-11-20 | 中国地质大学（武汉） | Method for measuring tensile strength of hydrate deposit |
| CN115165652A (en) * | 2022-07-27 | 2022-10-11 | 中国科学院武汉岩土力学研究所 | Testing device for suction force of sludge soil matrix and implementation method thereof |
| CN114965142A (en) * | 2022-08-02 | 2022-08-30 | 中国科学院地质与地球物理研究所 | Device for testing soil-water characteristic curve of hydrate deposit |
| CN114965142B (en) * | 2022-08-02 | 2022-09-30 | 中国科学院地质与地球物理研究所 | Device for testing soil-water characteristic curve of hydrate deposit |
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