CN106596224A - Experimental apparatus and method for preparing natural gas hydrate rock sample via two-step process - Google Patents
Experimental apparatus and method for preparing natural gas hydrate rock sample via two-step process Download PDFInfo
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- CN106596224A CN106596224A CN201611152896.0A CN201611152896A CN106596224A CN 106596224 A CN106596224 A CN 106596224A CN 201611152896 A CN201611152896 A CN 201611152896A CN 106596224 A CN106596224 A CN 106596224A
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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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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/108—Production of gas hydrates
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L7/00—Fuels produced by solidifying fluid fuels
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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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Abstract
The invention an experimental apparatus and method for preparing a natural gas hydrate rock sample via two-step process; the apparatus according to its technical scheme comprises a cold storage, a reactor, a confining pressure pump, a gas supply system, a computer data collection system and the like; all experimental systems are positioned in the low-temperature cold storage, and cold storage temperature is adjusted through a temperature control system of the cold storage; the output end of the confining pressure pump is connected with the reactor; the output end of the gas supply system is connected with the reactor; a gas flowmeter and a temperature sensor are connected with the computer data collection system. The method for preparing the natural gas hydrate rock sample via two-step process comprises the steps of first, generating hydrate in a rock sample; second, decreasing methane gas pressure to around phase equilibrium pressure but slightly higher than phase equilibrium pressure so that the hydrate is recrystallized. By using the apparatus and method, the problem in the preparation of natural gas hydrate rock samples is solved, a hydrate rock sample closer to an actual hydrate reservoir in physical mechanical characteristic can be acquired, and experimental support is provided for the drilling and development of natural gas hydrate resources.
Description
Technical field
The present invention relates to a kind of Gas Hydrate Drilling development field, more particularly to a kind of two-step method prepares gas water
The experimental provision and method of compound rock sample.
Background technology
China is energy-consuming state maximum in the world, and energy consumption accounts for the 23% of the whole world, while China's energy utilization rate
Low, unbalance of structure is less as the natural gas proportion of clean energy resource, compares higher shared by oil, coal, in recent years global gas
Waiting change causes people to pay much attention to, and low-carbon energy-saving, Optimization of Energy Structure, development clean energy resource is imperative.Natural gas is hydrated
Thing is the crystalline compounds of natural gas and water molecules, and it has, and stock number is big, energy density is high and low stain etc. is excellent
Point, is acknowledged as the important follow-up clean energy resource with good prospect, realizes that the exploitation of natural gas hydrate resources are right
In the energy industry development of propulsion China, improve energy consumption structure, ensure energy security supply, promote Ecological Civilization Construction, protect
Hold the sustainable development of socio-economy significant.Meanwhile, planned according to state key research and development, carry out gas hydrates examination
Adopt the important energy source become during 13 strategic.Limited by hydrate phase balance condition, gas hydrates can only be in height
Force down and exist under temperature, it is difficult to hydrate formation rock core is got in original position.During boring and coring, the change of load can cause hydration
The disturbance of thing earth formation, the change of pressure and temperature can also make partially hydrated thing decompose, and the core of acquirement can not be true
Reflection hydrate formation physico mechanical characteristic.Thus at present the experimental study of hydrate formation is mainly closed by laboratory
Into synthetic core sample containing hydrate carry out dependence test.
In recent years, it is to experience unrestrained in sedimentation environment by hydrate although being manually prepared for rock sample containing hydrate
What long period was formed, depositional environment is complicated, and indoor preparation is Fast back-projection algorithm, synthesis condition also differ with actual formation compared with
Greatly.As Application No. CN201110353136.7 patent of invention announce hydrate sediment in-situ preparation with decomposition and its ooze
Thoroughly rate measures integrated apparatus, although can complete fabricated in situ and the test of hydrate sediment, but hydrate is advanced when preparing
Row pressurization prepares rock sample skeleton and is input into methane gas and water again and generates hydrate in rock sample hole, and this is with partially hydrated thing with stratum
Physical condition in the form of skeleton is not inconsistent, while being difficult to the realization of precise control hydrate concentration yet；It is prepared by the invention
It is that methane and hydrate rapid crystallization generation hydrate are made in the case of degree of supercooling is great during hydrate, and in actual formation then
It is the slow hydrate for generating under the pressure and temperature of close phase balance condition, and degree of supercooling is bigger, and hydrate can be affected brilliant
The tissue topography of body and crystalline types, make the lattice of artificial hydrate sample cementing for machinery, rather than the lattice of actual formation
Cementing form, these can cause the physico mechanical characteristic containing hydrate rock sample for preparing to differ larger with actual reservoir.
For the requirement for meeting natural gas hydrate resources probing and develop, accurately obtain and actual formation physico mechanical characteristic
Hydrate synthetic core sample the most close, need develop can truly reflect the hydrate people of hydrate formation physico mechanical characteristic
Lithogenesis sample preparation method.
The content of the invention
The purpose of the present invention is aiming at the drawbacks described above of prior art presence, there is provided a kind of two-step method prepares gas water
The experimental provision and method of compound rock sample, is prepared with obtaining the hydrate rock sample being more nearly with actual formation physico mechanical characteristic
Method, the probing and exploitation for natural gas hydrate resources provides experiment and supports.
A kind of two-step method that the present invention is mentioned prepares the experimental provision of gas hydrates rock sample, freezer（1）It is interior to install anti-
Answer kettle（2）, methane gas cylinder（3）, gas flowmeter（6）, reclaim air bag（15）, confined pressure pump（17）, computer data acquisition system
（21）, the first atmospheric valve（14）, the second atmospheric valve（19）, freezer（1）The temperature control of -20 DEG C ~ room temperature is capable of achieving,
The methane gas cylinder（3）Jing pressure-reducing valves（4）Pass through the first high pressure line afterwards（11）With reactor（2）It is connected, for examination
The generation of hydrate in sample provides methane；
Confined pressure pump（17）By the second high pressure line（16）With reactor（2）It is connected, for reactor（2）In sample apply
Confined pressure；
First atmospheric valve（14）Installed in the 3rd high pressure line（12）On, and by the 3rd high pressure line（12）With reactor（2）
It is connected, for reactor（2）In methane be vented；
Second atmospheric valve（19）Installed in the 6th high pressure line（18）On, and by the 6th high pressure line（18）With reactor（2）
It is connected, for reactor（2）Middle confined pressure fluid is vented；
Second stop valve（10）It is mounted in the 4th high pressure line（22）On, the 4th high pressure line（22）One end and the first high pressure line
（11）It is connected, the other end and the 3rd high pressure line（12）It is connected, for realizing that sample two ends supply simultaneously；
First data transmission line（7）One end and gas flowmeter（6）It is connected, the other end and computer data acquisition system（21）
It is connected, for realizing the real-time monitoring to methane flow；
Second data line（20）One end and temperature sensor（29）It is connected, the other end and computer data acquisition system
（21）It is connected, for realizing generating hydrate and the real-time monitoring decomposed.
Preferably, aforesaid reaction vessel（2）Including push-down head（23）, seaming chuck（26）, the first seepage flow pad（27）, the second seepage flow
Pad（28）, rock sample oil removal set（24）, rock sample（25）It is clipped in push-down head（23）And seaming chuck（26）Between, rock sample（25）With push-down head
（23）Between the first seepage flow pad is installed（27）, rock sample（25）With seaming chuck（26）Between the second seepage flow pad is installed（26）, use
To prevent sedimentary particle from coming off blocking pipeline；Rock sample oil removal set（24）Positioned at rock sample（25）Outside, for realizing to rock sample hole
The separation of pressure system and confined pressure system.
Preferably, above-mentioned seaming chuck（26）Two circular channels are inside provided with, one of circular channel is to realize methane
From rock sample（25）End face flow out；Another circular channel is used for placing temperature sensor（29）.
Preferably, above-mentioned seaming chuck（26）Lower surface section on process fluted, be easy to methane in rock sample（25）Outlet
The flowing of end face.
Preferably, above-mentioned push-down head（23）Centre be provided with a circular channel, methane is delivered to into rock sample（25）
In, the flowing of methane gas is realized, realize uniform supply.
Preferably, above-mentioned push-down head（23）Upper surface section upper band it is fluted, be easy to methane gas in rock sample（25）Enter
The flowing of mouth end face.
A kind of two-step method that the present invention is mentioned prepares the using method of the experimental provision of gas hydrates rock sample, its preparation
Process is carried out in two steps, the first step, and hydrate, second step, by methane gas reduced pressure to the pressure that balances each other are generated in rock sample
Power nearby but slightly above vapor pressure, makes lattice activity aggravation, and lattice form is closer with actual reservoir.
A kind of two-step method that the present invention is mentioned prepares the using method of the experimental provision of gas hydrates rock sample, concrete real
Test step as follows：
（1）According to mineral composition and hydrate concentration sand, the soil and powder of actual formation in subzero low temperature environment
Shape distilled water ice cube is pressed into the skeleton of rock sample；
（2）Rock sample outside is superscribed into rock sample oil removal set（24）It is placed in reactor（2）It is interior；
（3）Open confined pressure pump（17）, make reactor（2）In full of low temperature resistant fluid and applying 0.5MPa confined pressures；
（4）Open the second stop valve（10）, the 3rd stop valve（13）With vacuum block valve（9）Rock sample hole is vacuumized；
（5）Open the first stop valve（5）, using methane gas cylinder（3）Rock sample is supplied, increases pore pressure, while utilizing
Confined pressure pump（17）Increase confined pressure, utilize and push-down head（23）Connected servo-control system adds axle pressure, remains that confined pressure is more than
More than gas pressure 0.5MPa, when pressure reaches setting value, maintains confined pressure, axle pressure and gas pressure constant；
（6）Temperature of ice house is slowly increased to more than 0 DEG C, keeps confined pressure, axle pressure and gas pressure constant, methane and water generating are hydrated
Thing；
（7）Work as gas flowmeter（6）When accumulative reading no longer changes, maintain 24 hours, hydrate is generated completely；
（8）Gas pressure is reduced to hydrate Critical Stability pressure above 0.1MPa according to hydrate phase balance curve, 12 are kept
Hour, make crystal of hydrate form from just generate when the mechanical cementing lattice that is changed into it is cementing, rock sample containing hydrate preparation finish.
Preferably, the diameter 25mm of above-mentioned rock sample, height 50mm.
The present invention compared with prior art, has the advantages that：
(1), the present invention solves the problems, such as that part hydrate is with bound form in artificial natural gas hydrate reservoir rock sample,
Simultaneously hydrate is generated under actual crustal stress states, it is more close with actual reservoir；
(2), by two-step method, hydrate is recrystallized near vapor pressure, makes the lattice types and reality of hydrate rock sample
Border reservoir is more close, more guiding to hydrate reservoir Related Experimental Study；
(3), hydrate is generated by the way of the supply of two ends, reduces the spilling of fluid, make the calculating of hydrate concentration more
Accurately；
(4）, the present invention main equipment be on original hydrate fabricated in situ and rock mechanics triaxial tests Equipment Foundations
Transform and come, greatly save equipment cost, requirement of experiment can be met again；
(5), the gas hydrates synthesis to seabed and frozen soil field can be simulated well, to gas hydrates thing
The research of reason mechanical characteristic has great impetus.
Description of the drawings
Fig. 1 is the experimental provision schematic diagram that two-step method of the present invention prepares gas hydrates rock sample；
Fig. 2 is reactor internal structure schematic diagram；
Fig. 3 is seaming chuck schematic diagram in reactor；
Fig. 4 is the upward view in Fig. 3；
Fig. 5 is push-down head schematic diagram in reactor；
Fig. 6 is the top view in Fig. 5；
In figure, 1, freezer, 2, reactor, 3, methane gas cylinder, 4, pressure-reducing valve, the 5, first stop valve, 6, gas flowmeter, 7, first
Data line, the 8, the 5th high pressure line, 9, vacuum block valve, the 10, second stop valve, the 11, first high pressure line, the 12, the 3rd
High pressure line, the 13, the 3rd stop valve, the 14, first atmospheric valve, 15, reclaim air bag, the 16, second high pressure line, 17, confined pressure pump,
18th, the 6th high pressure line, the 19, second atmospheric valve, the 20, second data line, the 21, computer data acquisition system, the 22, the 4th
High pressure line, 23, push-down head, 24, oil removal set, 25, rock sample, 26, seaming chuck, the 27, first seepage flow pad, the 28, second seepage flow pad,
29th, temperature sensor.
Specific embodiment
As shown in figure 1, two-step method prepares the experimental provision of gas hydrates rock sample, install in freezer 1 reactor 2,
Methane gas cylinder 3, gas flowmeter 6, recovery air bag 15, confined pressure pump 17, computer data acquisition system 21, the first atmospheric valve 14,
Second atmospheric valve 19 etc..
The methane gas cylinder is connected by the first high pressure line 11 Jing after pressure-reducing valve 4 with reactor 2, for water in sample
The generation of compound provides methane；
Confined pressure pump 17 is connected by the second high pressure line 16 with reactor 2, for applying confined pressure to the sample in reactor 2；
Freezer 1 is capable of achieving the temperature control of -20 DEG C ~ room temperature, and all experimental facilities and experimentation are carried out in freezer；
First atmospheric valve 14 is arranged on the 3rd high pressure line 14, and is connected with reactor 2 by the 3rd high pressure line 14, is used for
Methane in reactor 2 is vented；
Second atmospheric valve 19 is arranged on the 6th high pressure line 18, and is connected with reactor 2 by the 6th high pressure line 18, is used for
Confined pressure fluid in reactor 2 is vented；
First stop valve 10 is mounted on the 4th high pressure line 22, one end and the phase of the first high pressure line 11 of the 4th high pressure line 22
Even, the other end is connected with the 3rd high pressure line 12, for realizing that sample two ends supply simultaneously；
One end of first data transmission line 7 is connected with gas flowmeter 6, and the other end is connected with computer data acquisition system 21,
For realizing the real-time monitoring to methane flow；
One end of second data line 20 is connected with temperature sensor 29, the other end and the phase of computer data acquisition system 21
Even, the real-time monitoring for realizing generating hydrate and decomposing（Decomposition of hydrate is absorbed heat, and hydrate generates heat release）.
As shown in Fig. 2 the reactor 2 includes：Push-down head 23, seaming chuck 26, the first seepage flow pad 27, the second seepage flow pad
28, rock sample oil removal set 24.Rock sample 25 is clipped between push-down head 23 and seaming chuck 26, and is provided between rock sample 25 and push-down head 23
One seepage flow pad 27, is provided with the second seepage flow pad 26 between rock sample 25 and seaming chuck 26, for preventing sedimentary particle from coming off blocking
Pipeline.Rock sample oil removal set 24 is located at the outside of rock sample 25, for realizing to rock sample pore pressure system（Methane）With the separation of confined pressure system
It is independent.
As shown in Figure 3-4, two circular channels are provided with seaming chuck 26, one of passage is to realize methane from rock sample
25 end face flows out；Another passage is used for placing temperature sensor 29；It is machined with the lower surface section of seaming chuck 26 multiple
Groove, is easy to methane to combine for eight deep-slotted chip breakers of a quarter size in the flowing of the exit end face of rock sample 25, and above-mentioned groove
Into two circular configurations.
As seen in figs. 5-6, the centre of push-down head 23 is provided with a circular channel, methane is delivered in rock sample 25,
Realize the flowing of methane gas；The upper surface section upper band of push-down head 23 is fluted, is easy to methane gas in the arrival end of rock sample 25
The flowing in face, and above-mentioned groove is combined into two circular configurations for eight deep-slotted chip breakers of a quarter size.
The two-step method that the present invention is mentioned prepares the using method of the experimental provision of gas hydrates rock sample, its preparation process
It is carried out in two steps, the first step, hydrate is generated in rock sample, second step is attached to vapor pressure by methane gas reduced pressure
Near but slightly above vapor pressure, makes lattice activity aggravation, and lattice form is closer with actual reservoir.
The specific experiment step of the present invention is as follows：
（1）In subzero low temperature environment（This experiment is -5 DEG C）Mineral composition and hydrate saturation according to actual formation
Degree sand, soil and powder shaped distillation water-ice block are with certain mass ratio（This experiment is 1:1:0.5）It is pressed into rock sample skeleton.
The diameter 25mm of rock sample, height 50mm.
（2）The rock sample for suppressing outside is superscribed into rock sample oil removal set 24 to be placed in reactor 2.
（3）Confined pressure pump 17 is opened, makes low temperature resistant fluid to be full of in reactor 2 and applies 0.5MPa confined pressures.
（4）Open the second stop valve 10, the 3rd stop valve 13 and vacuum block valve 9 rock sample hole is carried out vacuumizing 1 it is little
When.
（5）The first stop valve 5 is opened, rock sample is supplied using methane gas cylinder 3, increase rock sample pore pressure, while
Increase confined pressure using confined pressure pump 17, using the servo-control system being connected with push-down head 23 axle pressure is added, remain that confined pressure is more than
More than gas pressure 0.5MPa, when pressure reaches setting value（According to the reservoir conditions of this experimental simulation, methane air pressure is set
Power is 10MPa, and axle presses 14MPa, confined pressure 12MPa）, maintain confined pressure, axle pressure and gas pressure constant.
（6）Temperature of ice house is slowly increased to more than 0 DEG C（This experiment is set as 5 DEG C）, keep confined pressure and gas pressure not
Change, methane and water generating hydrate.
（7）When gas flowmeter 6 adds up reading no longer to change, maintain 24 hours, it is believed that hydrate is complete
It is complete to generate, using the change calculations hydrate concentration of gas flow count value, with the hydrate using ice cube Mass Calculation
Saturation degree is mutually corrected.
（8）Gas pressure is reduced to hydrate Critical Stability pressure above 0.1MPa according to hydrate phase balance curve（Such as
This experimental temperature is 5 DEG C, and critical pressure is 4.2MPa, then reduce pressure to 4.3MPa）If other decomposition pressures are unknown
During hydrate, temperature sensor 29 and gas flowmeter 6 can be paid close attention to the moment, if temperature changes or pressure flow becomes extremely
Change, illustrate that hydrate starts to decompose, then stop being depressured and increasing 0.1MPa pressure）Kept for 12 hours, make crystal of hydrate form
The mechanical cementing lattice that is changed into when just generating is cementing, and rock sample containing hydrate is prepared and finished.
The above, is only the part preferred embodiment of the present invention, and any those of ordinary skill in the art may profit
The technical scheme being equal to is changed or is revised as with the technical scheme of above-mentioned elaboration.Therefore, according to the technology of the present invention
Any simple modification or substitute equivalents that scheme is carried out, belong to the greatest extent the scope of protection of present invention.
Claims (9)
1. a kind of two-step method prepares the experimental provision of gas hydrates rock sample, it is characterized in that：Freezer（1）Interior installation reactor
（2）, methane gas cylinder（3）, gas flowmeter（6）, reclaim air bag（15）, confined pressure pump（17）, computer data acquisition system（21）、
First atmospheric valve（14）, the second atmospheric valve（19）, freezer（1）The temperature control of -20 DEG C ~ room temperature is capable of achieving,
The methane gas cylinder（3）Jing pressure-reducing valves（4）Pass through the first high pressure line afterwards（11）With reactor（2）It is connected, for examination
The generation of hydrate in sample provides methane；
Confined pressure pump（17）By the second high pressure line（16）With reactor（2）It is connected, for reactor（2）In sample apply
Confined pressure；
First atmospheric valve（14）Installed in the 3rd high pressure line（12）On, and by the 3rd high pressure line（12）With reactor（2）
It is connected, for reactor（2）In methane be vented；
Second atmospheric valve（19）Installed in the 6th high pressure line（18）On, and by the 6th high pressure line（18）With reactor（2）
It is connected, for reactor（2）Middle confined pressure fluid is vented；
Second stop valve（10）It is mounted in the 4th high pressure line（22）On, the 4th high pressure line（22）One end and the first high pressure line
（11）It is connected, the other end and the 3rd high pressure line（12）It is connected, for realizing that sample two ends supply simultaneously；
First data transmission line（7）One end and gas flowmeter（6）It is connected, the other end and computer data acquisition system（21）
It is connected, for realizing the real-time monitoring to methane flow；
Second data line（20）One end and temperature sensor（29）It is connected, the other end and computer data acquisition system
（21）It is connected, for realizing generating hydrate and the real-time monitoring decomposed.
2. two-step method according to claim 1 prepares the experimental provision of gas hydrates rock sample, it is characterized in that：It is described anti-
Answer kettle（2）Including push-down head（23）, seaming chuck（26）, the first seepage flow pad（27）, the second seepage flow pad（28）, rock sample oil removal set
（24）, rock sample（25）It is clipped in push-down head（23）And seaming chuck（26）Between, rock sample（25）With push-down head（23）Between be provided with
One seepage flow pad（27）, rock sample（25）With seaming chuck（26）Between the second seepage flow pad is installed（26）, for preventing sedimentary particle
Come off blocking pipeline；Rock sample oil removal set（24）Positioned at rock sample（25）Outside, for realizing to rock sample pore pressure system and confined pressure system
Separation.
3. two-step method according to claim 1 prepares the experimental provision of gas hydrates rock sample, it is characterized in that：On described
Pressure head（26）Two circular channels are inside provided with, one of circular channel is to realize methane from rock sample（25）End face flow out；
Another circular channel is used for placing temperature sensor（29）.
4. two-step method according to claim 1 prepares the experimental provision of gas hydrates rock sample, it is characterized in that：It is described
Seaming chuck（26）Lower surface section on process fluted, be easy to methane in rock sample（25）The flowing of exit end face.
5. two-step method according to claim 1 prepares the experimental provision of gas hydrates rock sample, it is characterized in that：Under described
Pressure head（23）Centre be provided with a circular channel, methane is delivered to into rock sample（25）In, the flowing of methane gas is realized,
Realize uniform supply.
6. two-step method according to claim 1 prepares the experimental provision of gas hydrates rock sample, it is characterized in that：Under described
Pressure head（23）Upper surface section upper band it is fluted, be easy to methane gas in rock sample（25）The flowing of entrance face.
7. a kind of two-step method as any one of claim 1-6 prepares making for the experimental provision of gas hydrates rock sample
With method, it is characterized in that preparation process is carried out in two steps, the first step generates hydrate, second step, by methane gas in rock sample
Reduced pressure makes lattice activity aggravation, lattice form and actual reservoir to vapor pressure nearby but slightly above vapor pressure
It is closer.
8. a kind of two-step method as any one of claim 1-6 prepares making for the experimental provision of gas hydrates rock sample
With method, it is characterized in that specific experiment step is as follows：
（1）According to mineral composition and hydrate concentration sand, the soil and powder of actual formation in subzero low temperature environment
Shape distilled water ice cube is pressed into the skeleton of rock sample；
（2）Rock sample outside is superscribed into rock sample oil removal set（24）It is placed in reactor（2）It is interior；
（3）Open confined pressure pump（17）, make reactor（2）In full of low temperature resistant fluid and applying 0.5MPa confined pressures；
（4）Open the second stop valve（10）, the 3rd stop valve（13）With vacuum block valve（9）Rock sample hole is vacuumized；
（5）Open the first stop valve（5）, using methane gas cylinder（3）Rock sample is supplied, increases pore pressure, while utilizing
Confined pressure pump（17）Increase confined pressure, utilize and push-down head（23）Connected servo-control system adds axle pressure, remains that confined pressure is more than
More than gas pressure 0.5MPa, when pressure reaches setting value, maintains confined pressure, axle pressure and gas pressure constant；
（6）Temperature of ice house is slowly increased to more than 0 DEG C, keeps confined pressure, axle pressure and gas pressure constant, methane and water generating are hydrated
Thing；
（7）Work as gas flowmeter（6）When accumulative reading no longer changes, maintain 24 hours, hydrate is generated completely；
（8）Gas pressure is reduced to hydrate Critical Stability pressure above 0.1MPa according to hydrate phase balance curve, 12 are kept
Hour, make crystal of hydrate form from just generate when the mechanical cementing lattice that is changed into it is cementing, rock sample containing hydrate preparation finish.
9. two-step method according to claim 8 prepares the using method of the experimental provision of gas hydrates rock sample, and it is special
Levying is：The diameter 25mm of described rock sample, height 50mm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107462508A (en) * | 2017-08-16 | 2017-12-12 | 西南石油大学 | A kind of multi- scenarios method seepage flow multifunction experiment apparatus and method of testing |
| CN107621431A (en) * | 2017-09-25 | 2018-01-23 | 华南理工大学 | A kind of rapid measurement device and method of the hydrate concentration suitable for the hydrate sediment of a variety of coring devices |
| CN108918183A (en) * | 2018-09-19 | 2018-11-30 | 吉林大学 | Micro- brill experimental provision and method are turned round in hydrate vibration in ocean |
| CN109827829A (en) * | 2019-04-09 | 2019-05-31 | 大连理工大学 | A kind of preparation of cycle type hydrate sediment sample and dynamic characteristic test apparatus |
| CN110118678A (en) * | 2019-04-19 | 2019-08-13 | 湖北理工学院 | A kind of sample making apparatus of soil containing gas hydrates and its at quadrat method |
| RU2726756C1 (en) * | 2019-09-26 | 2020-07-15 | федеральное государственное бюджетное образовательное учреждение высшего образования "Кузбасский государственный технический университет имени Т.Ф. Горбачева" (КузГТУ) | Method of determining amount of gas hydrate formed in natural coal |
| CN112748011A (en) * | 2019-10-31 | 2021-05-04 | 中国石油大学(华东) | Device and method for testing mechanical characteristics of contact surface of marine energy soil containing natural gas hydrate and structure |
| CN117468878A (en) * | 2023-11-01 | 2024-01-30 | 四川大学 | Deep sea natural gas hydrate low-disturbance coring experiment platform and use method thereof |
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| CN107462508A (en) * | 2017-08-16 | 2017-12-12 | 西南石油大学 | A kind of multi- scenarios method seepage flow multifunction experiment apparatus and method of testing |
| CN107621431A (en) * | 2017-09-25 | 2018-01-23 | 华南理工大学 | A kind of rapid measurement device and method of the hydrate concentration suitable for the hydrate sediment of a variety of coring devices |
| CN107621431B (en) * | 2017-09-25 | 2023-10-31 | 华南理工大学 | Device and method for rapidly measuring hydrate saturation in hydrate sediment suitable for various coring devices |
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| CN112748011A (en) * | 2019-10-31 | 2021-05-04 | 中国石油大学(华东) | Device and method for testing mechanical characteristics of contact surface of marine energy soil containing natural gas hydrate and structure |
| CN117468878A (en) * | 2023-11-01 | 2024-01-30 | 四川大学 | Deep sea natural gas hydrate low-disturbance coring experiment platform and use method thereof |
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