CN106840911A - A kind of liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision and method - Google Patents
A kind of liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision and method Download PDFInfo
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Abstract
It is of the invention to be connected with temperature-control pressure-control device by low temperature resistant metal pipe line from supercharging liquid nitrogen container the present invention relates to a kind of liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision and method, ultra-low temperature liquid nitrogen is housed from supercharging liquid nitrogen container inside；The high-pressure nitrogen bottle is connected with temperature-control pressure-control device and freezing-thawing damage device upper end respectively by gases at high pressure pipeline, and high-pressure nitrogen bottle is built with high pressure nitrogen；The bottom of temperature-control pressure-control device is connected by low temperature resistant metal pipe line with the bottom of freezing-thawing damage device；Shale core is provided with inside the freezing-thawing damage device, and is connected with data collecting system by low temperature foil gauge.Beneficial effect is：The present invention can carry out the shale freezing-thawing damage experiment under different temperatures, the effect of pressure liquid nitrogen, adjustable temperature scope is big, can true simulated formation rock contacted with liquid nitrogen after damage deterioration condition, experimental technique is simple, experimental error is small, for very low temperature flow fracturing technique exploitation shale gas reservoir provides scientific basis and theoretical foundation.
Description
Technical field
The present invention relates to a kind of petroleum works reservoir stimulation transformation field, more particularly to a kind of liquid nitrogen temperature-control pressure-control freeze thawing is damaged
Hinder shale experimental provision and method, after the design of hydraulic fracturing scheme and construction for ultra-low temperature liquid nitrogen fracturing technique exploitation shale gas
Reservoir productivity is predicted.
Background technology
Energy crisis and environmental problem are the biggest threats that world today's human development faces, and environmental problem is in very great Cheng
Caused by energy consumption structure is unreasonable on degree.Resources Reserve based on coal, determines the energy of the China based on coal
Consumption structure, in China's primary energy consumption structure, coal has accounted for 69%, and about 40% is higher by than world average level；And day
Right gas only accounts for 5%, the world average level far below 24%.Increase the ratios of the clean energy resource in energy consumption structure such as natural gas
Example, for optimization China energy resource structure, reduces domestic production of units total value CO2Discharge is significant.In recent years, with me
Social economy of state grows continuously and fast, and the demand of the energy hits new peak repeatly, and traditional petroleum resources increasingly depleted, causes China in addition
Oil, natural gas external dependence degree constantly rise.Dependence on foreign countries for oil 1.2% was risen violently by 2013 by 1993
58.1%, natural gas external dependence degree also by 2006 0.8% it is rapid rise to 2013 31.6%.It was predicted that arriving the year two thousand twenty
The average annual consumption figure of Natural Gas In China will be up to 3000 × 108m3, and China's natural gas yield is only 2000 × 108m when the time comes3Left and right.Cause
This, accelerates the exploration and development of unconventional gas resource, for ensuring that national energy strategic security has great importance.
The shale gas annual production only 100 × 108m of north America region in 20003, reached to this area's shale gas annual production in 2010
To 1500 × 108m3, 15 times are increased between 10 years." the shale gas revolution " started by North America has greatly shaken global traditional energy
Source domain, excites national governments and oil gas/energy company passion beyond imagination to shale gas resource.The success in the U.S. is opened
Hair experience have shown that, only fully exposure reservoir area, a large amount of release adsorbed gas reserves link up whole reservoir, could improve
Single well productivity realizes commercial development, has thus sprouted brand-new shale gas fracturing technique " volume fracturing ".Shale gas reservoir volume
Pressure break refers to during hydraulic fracturing, intrinsic fracture is constantly expanded, and brittle rock constantly produces shearing slip, forms day
Right crack and the interlaced fracture network of man-made fracture, so as to increase transformation volume, improve gas yield and ultimate recovery.
Since 2005, although China is in succession in south of Sichuan Basin, China Paleozoic group, North of Sichuan Basin Mesozoic Era, Ordos Basin three
The breakthrough that shale gas are prospected is achieved in multiple areas such as folded system and the marine facies in multiple epoch, terrestrial facies richness organic shale, but
Substantial amounts of mining site practice have shown that:China's shale gas reservoir is difficult to carry out extensive volume fracturing, reservoir reconstruction finite volume, individual well
Yield poorly so that the prospect of this industry causes anxiety.Contrast Sino-U.S.'s Shale Gas Accumulation and occurrence condition, discovery form this challenge
Main cause is as follows：1. reservoir buried depth is big（U.S.'s shale buried depth is general at 200-2000 meters, and China's overwhelming majority shale buried depth exceedes
3000 meters, part is even more than 5000m）；2. the brittle mineral content such as quartz is low so that shale fragility is generally less than U.S.'s allusion quotation
Type shale reservoir；3. great burying causes that temperature is high, confined pressure is big so that the deformation of shale is substantially from fragility to ductility transition；4. layer
Interior horizontal ground stress deviation is big, and the ability for forming seam net is low；5. intrinsic fracture agensis.These features significantly limit complexity and split
The formation of network is stitched, volume fracturing correctional effect is drastically influence.These unique reservoir geology power for China's shale gas reservoir
Feature is learned, is explored and is improved stratum compressibility, form the new method of complex fracture network, as current shale gas reservoir Efficient Development urgently
The key issue that need to be solved.
Ultra-low temperature liquid nitrogen fracturing technique refers to that liquid nitrogen is injected into a kind of novel anhydrous of reservoir as fracturing fluid on ground
Fracturing technique.The liquefied gas at low temp such as liquid nitrogen, generally with extremely low temperature (LN2- 195.8 DEG C of normal boiling point), connect when with rock
When touching, rock surface temperature decrease can be made, high speed contraction distortion occurs, form a large amount of microfissures；Additionally, freezing process mesopore
It is same with the frost-heave force that the water in crack mutually becomes ice generation that rock interior can be caused to damage.Bad effect of the liquid nitrogen to shale
Stronger, reservoir is broken more abundant after pressure break, and the passage of fluid neuron network and migration is more, and reservoir reconstruction effect is also better.At present, close
Mostly launch around cold regions engineering Frozen soil problems in the research of rock freezing-thawing damage problem, temperature only has tens degree, and does not apply to
In the situation of a few Baidu's temperature gradients of nitrogen ultra low temperature fluid.
The experimental provision of freezing-thawing damage is carried out to shale therefore, need develop and can regulate and control different temperatures, pressure liquid nitrogen, is
The reservoir productivity prediction that ultra-low temperature liquid nitrogen fracturing technique is developed after shale gas reservoir design of hydraulic fracturing scheme and pressing crack construction provide according to
According to.
The content of the invention
The drawbacks described above that the purpose of the present invention exists aiming at prior art, there is provided a kind of liquid nitrogen temperature-control pressure-control freeze thawing is damaged
Hinder shale experimental provision and method, be ultralow temperature liquid to realize that damage of the shale under the effect of different temperatures pressure liquid nitrogen is deteriorated
Nitrogen fracturing technique exploitation shale gas reservoir provides scientific basis and theoretical foundation.
A kind of liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision that the present invention is mentioned, including supercharging liquid nitrogen container certainly（1）、
Temperature-control pressure-control device（2）, freezing-thawing damage device（5）, high-pressure nitrogen bottle（4）, data collecting system；Certainly the supercharging liquid nitrogen container
（1）By low temperature resistant metal pipe line（7）With temperature-control pressure-control device（2）It is connected, low temperature resistant metal pipe line（7）On liquid feed valve is installed
（12）With ultralow temperature flowmeter（11）, from supercharging liquid nitrogen container（1）Inside is equipped with ultra-low temperature liquid nitrogen；The high-pressure nitrogen bottle（4）It is logical
Cross high pressure gas fluid line（27）Respectively with temperature-control pressure-control device（2）With freezing-thawing damage device（5）Upper end connects, high-pressure nitrogen bottle
（4）Built with high pressure nitrogen；The temperature-control pressure-control device（2）Top temperature-control pressure-control device upper end cover is installed（24）, temperature control
Pressure control device（2）Bottom pass through low temperature resistant metal pipe line（7）With freezing-thawing damage device（5）Bottom connection, temperature-control pressure-control dress
Put（2）Tapping valve is provided with lower part outlet（29）；
The freezing-thawing damage device（5）Inside is provided with one or more shale core（6）, shale core（6）It is provided with
Low temperature foil gauge（61）, and by low temperature foil gauge（61）With the strain testing instrument of data collecting system（9）Connection, damages in freeze thawing
Hinder device（5）Top be provided with freezing-thawing damage device upper end cover（54）, bottom is provided with and low temperature resistant metal pipe line（7）What is connected goes out
Mouthful；
The data collecting system includes four-way temperature, pressure digital display（3）, acoustic emission detector（8）, strain testing
Instrument（9）And computer（10）, wherein, acoustic emission detector（8）With strain testing instrument（9）Monitoring Data is by computer（10）It is responsible for
Record.
Preferably, above-mentioned temperature-control pressure-control device（2）It is divided into inside and outside two-layer, its internal layer is the first deep cooling steel inner bag（22）, it is outer
Layer is the first polyurethane adiabatic layer（21）, and the first polyurethane adiabatic layer（21）By temperature-control pressure-control device upper end cover（24）It is wrapped in
It is interior, temperature-control pressure-control device（2）Bottom inner bag and outer layer between be provided with heating plate（23）, temperature-control pressure-control device（2）Top
Temperature-control pressure-control device upper end cover（24）Ultralow temperature temperature sensor is installed（25）, pressure sensor（26）And atmospheric valve（28）.
Preferably, above-mentioned temperature-control pressure-control device upper end cover（24）It is made up of top cover and column, the outer ring of top cover is provided with first
Convex edge, the first convex edge is provided with screw, by the first sealing bolt（241）With temperature-control pressure-control device（2）It is fixed；Described first is convex
The lower surface on edge is provided with the first Graphite pad（242）, it is resistance to low that the column outer wall below the first convex edge is provided with the first polyurethane
Warm O-ring（243）, formed multi-stage sealed.
Preferably, above-mentioned freezing-thawing damage device（5）It is divided into inside and outside two-layer, its internal layer is the second deep cooling steel inner bag（52）, outward
Layer is the second polyurethane adiabatic layer（51）, and the second polyurethane adiabatic layer（51）By freezing-thawing damage device upper end cover（54）It is wrapped in
It is interior, the freezing-thawing damage device upper end cover at top（54）On the second ultralow temperature temperature sensor is installed（55）, second pressure sensing
Device（56）, acoustic emission sensor（58）, control pressure valve（53）With low temperature foil gauge wire（59）.
Preferably, above-mentioned freezing-thawing damage device upper end cover（54）It is made up of top cover and column, the outer ring of top cover is provided with second
Convex edge, the second convex edge is provided with screw, by the second sealing bolt（541）With freezing-thawing damage device（5）It is fixed；Described second is convex
The lower surface on edge is provided with the second Graphite pad（542）, it is resistance to low that the column outer wall below the second convex edge is provided with the second polyurethane
Warm O-ring（543）, formed multi-stage sealed.
Preferably, above-mentioned four-way temperature and pressure digital display（3）Two-way respectively with temperature-control pressure-control device（2）The of top
One ultralow temperature temperature sensor（25）, first pressure sensor（26）Connection；Another two-way respectively with freezing-thawing damage device（5）Top
The second ultralow temperature temperature sensor（55）, second pressure sensor（56）Connection.
Preferably, above-mentioned high-pressure nitrogen bottle（4）Top be provided with pressure gauge（41）, pressure-reducing valve（42）With total air intake valve
（43）, and with gases at high pressure pipeline（27）Connection.
Preferably, above-mentioned temperature-control pressure-control device upper end cover（24）Top cover external diameter more than column diameter.
Preferably, above-mentioned freezing-thawing damage device upper end cover（54）Top cover external diameter more than column diameter.
A kind of experimental technique of liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision that the present invention is mentioned, specific steps are such as
Under：
(a), prepare rock core to be tested, using cabinet-type electric furnace by shale core（6）Preset temperature is heated to, is checked and is confirmed liquid nitrogen
Each valve is closed on temperature-control pressure-control freezing-thawing damage shale experimental provision and pipeline；
(b), open from supercharging liquid nitrogen container liquid feed valve（12）, to temperature-control pressure-control device（2）The interior a small amount of liquid nitrogen of filling is carried out to device
Precooling, opens temperature-control pressure-control device atmospheric valve（28）, wait in complete discharge device and close atmospheric valve after nitrogen；
C (), shale freezing-thawing damage are tested
1. open from supercharging liquid nitrogen container（1）On liquid feed valve（12）, to temperature-control pressure-control device（2）Interior filling liquid nitrogen, closes feed liquor
Valve；Open high-pressure nitrogen bottle（4）Pressure-reducing valve（42）, nitrogen pressure is adjusted to by default freeze thawing pressure according to pressure gauge；Open total
Air intake valve（43）With the first valve（271）, to temperature-control pressure-control device（2）Nitrogen is filled with, when four-way temperature, pressure numeral is aobvious
Show device（3）Display temperature-control pressure-control device（2）After interior air pressure reaches freeze thawing pressure, now, freeze thawing pressure is more than nitrogen at such a temperature
Saturated vapour pressure, its object is to ensure that liquid nitrogen is not vaporized in heating process；Close the first valve（271）；Open
Heating plate（23）, liquid nitrogen is heated, when liquid nitrogen temperature is close to default freeze thawing temperature, close heating plate（23）, using plus
Hot plate waste heat is heated to liquid nitrogen；Micro opening atmospheric valve（28）, air pressure is to freeze thawing pressure in slow regulation temperature-control pressure-control device
Power, the pressure that liquid nitrogen volumetric expansion is caused in elimination heating process rises；
2. by shale core（6）Taken out from cabinet-type electric furnace, stick low temperature resistant foil gauge（61）It is positioned over freezing-thawing damage device
（5）It is interior；Open the second valve（571）, to freezing-thawing damage device（5）Nitrogen is inside filled with, when air pressure reaches in freezing-thawing damage device
After freeze thawing pressure, total air intake valve is closed（43）, open the first valve（271）；Open temperature-control pressure-control device tapping valve（29）, root
According to law of connected vessels, liquid nitrogen is from temperature-control pressure-control device（2）Flow into freezing-thawing damage device（5）Until stream oriented device liquid level is identical；
In (d), shale frozen-thaw process, control pressure valve（53）Real-time monitoring freezing-thawing damage device（5）Interior gas pressure, eliminates
The pressure oscillation that liquid nitrogen vaporization is caused, it is ensured that freeze thawing pressure is fixed value；
After the completion of (e), shale frozen process experiment, the atmospheric valve of temperature-control pressure-control device is opened（28）Pressure release, takes out shale core, experiment
Finish.
Compared with prior art, its advantage is the present invention：
(1), experimental system is divided into two large divisions, liquid nitrogen temperature-control pressure-control and shale freeze thawing deterioration are carried out respectively, it is to avoid two parts
Between interfere, using heating plate and ultralow temperature temperature sensor accuracy controlling liquid nitrogen temperature, realize different cold shock temperature
Liquid nitrogen effect shale freezing-thawing damage experiment under degree；
(2), pressurizeed to liquid nitrogen using high-pressure nitrogen bottle, carry out the shale under different freeze thawing pressure and damage deterioration experiment, investigated and freeze
Melt the influence that pressure is damaged to the lower shale of liquid nitrogen effect；
(3), using cabinet-type electric furnace for rock core is heated, the temperature change in both direction is realized, investigates the identical temperature difference not equality of temperature
The degree influence that is damaged to shale of scope, actual response actual formation situation, for ultra-low temperature liquid nitrogen fracturing developing shale air lift
For the experimental result with actual directive significance；
(4), shale freeze thawing deterioration process is monitored in real time using two kinds of detection means of sound emission and foil gauge, is research page
Rock damage development process provides crucial experimental data；
(5), once can freeze thawing multiple rock cores, experiment rock core size is diameter 25mm, and 50mm high, experimental technique is simple, operation side
Just, experimental error is small.
Brief description of the drawings
Fig. 1 is the structural representation of liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision of the present invention；
Fig. 2 covers end view for temperature-control pressure-control device end；
Fig. 3 covers end view in section for temperature-control pressure-control device end
Fig. 4 is freeze thawing degradation device end cap upper surface schematic diagram；
Fig. 5 is the phasor of nitrogen；
In figure, 1- is pressurized liquid nitrogen container, 11- ultralow temperature flowmeters, 12- liquid feed valves, 2- temperature-control pressure-control devices, the poly- ammonia of 21- first certainly
Ester heat insulation layer, 22- the first deep cooling steel inner bags, 23- heating plates, 24 temperature-control pressure-control device upper end covers, the sealing bolts of 241- first,
The Graphite pads of 242- first, the low temperature resistant O-ring of the polyurethane of 243- first, 25- the first ultralow temperature temperature sensors, 26- the first surpasses
Low-temperature pressure sensor, 27- gases at high pressure pipelines, the valves of 271- first, 28- atmospheric valves, 29- tapping valves, 3- four-way channel temps
Pressure on the number display, 4- high-pressure nitrogen bottles, 41- pressure gauges, 42- pressure-reducing valves, the total air intake valves of 43-, 5- freezing-thawing damage devices,
The polyurethane adiabatics of 51- second layer, 52- the second deep cooling steel inner bags, 53- control pressure valves, 54- freezing-thawing damage device upper end covers,
The sealing bolts of 541- second, the Graphite pads of 542- second, the low temperature resistant O-ring of the polyurethane of 543- second, 55- the second ultralow temperature temperature
Sensor, 56- the second ultralow temperature pressure sensors, the valves of 571- second, 58- acoustic emission sensors, 59- low temperature foil gauges are led
Line, 6- shale cores, 61- low temperature foil gauges, the low temperature resistant metal pipe lines of 7-, 8- acoustic emission detectors, 9- strain testing instrument, 10-
Computer.
Specific embodiment
The preferred embodiments of the present invention are illustrated below in conjunction with accompanying drawing, it will be appreciated that preferred reality described herein
Apply example to be merely to illustrate and explain the present invention, be not intended to limit the present invention.
A kind of liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision that the present invention is mentioned, including supercharging liquid nitrogen container 1, control certainly
Temperature control pressure device 2, freezing-thawing damage device 5, high-pressure nitrogen bottle 4, data collecting system；It is described to pass through resistance to low from supercharging liquid nitrogen container 1
Warm metal pipe line 7 is connected with temperature-control pressure-control device 2, and liquid feed valve 12 and ultralow temperature flowmeter are provided with low temperature resistant metal pipe line 7
11, ultra-low temperature liquid nitrogen is housed from the inside of supercharging liquid nitrogen container 1；The high-pressure nitrogen bottle 4 by gases at high pressure pipeline 27 respectively with control
Temperature control pressure device 2 and the upper end of freezing-thawing damage device 5 connect, and high-pressure nitrogen bottle 4 is built with high pressure nitrogen；The temperature-control pressure-control device
2 top is provided with temperature-control pressure-control device upper end cover 24, and the bottom of temperature-control pressure-control device 2 is by low temperature resistant metal pipe line 7 and jelly
Melt the bottom connection of damaging device 5, tapping valve 29 is provided with the lower part outlet of temperature-control pressure-control device 2；
One or more shale core 6 is provided with inside the freezing-thawing damage device 5, shale core size is diameter
25mm, 50mm high；Shale core 6 is provided with low temperature foil gauge 61, and by low temperature foil gauge 61 and data collecting system should
Become tester 9 to connect, freezing-thawing damage device upper end cover 54 be provided with the top of freezing-thawing damage device 5, bottom be provided with it is low temperature resistant
The outlet of the connection of metal pipe line 7；
The data collecting system includes four-way temperature, pressure digital display 3, acoustic emission detector 8, the and of strain testing instrument 9
Computer 10, wherein, acoustic emission detector 8 is responsible for record with the Monitoring Data of strain testing instrument 9 by computer 10.
Referring to the drawings 1,2 and 3, a kind of 2 points of temperature-control pressure-control device that the present invention is mentioned is inside and outside two-layers, and its internal layer is first
Deep cooling steel inner bag 22, outer layer is the first polyurethane adiabatic layer 21, and the first polyurethane adiabatic layer 21 is by temperature-control pressure-control device upper end
Lid 24 is provided with heating plate 23, the top of temperature-control pressure-control device 2 in being wrapped between the bottom inner bag and outer layer of temperature-control pressure-control device 2
The temperature-control pressure-control device upper end cover 24 in portion is provided with ultralow temperature temperature sensor 25, pressure sensor 26 and atmospheric valve 28.
Wherein, temperature-control pressure-control device upper end cover 24 is made up of top cover and column, and the outer ring of top cover is provided with the first convex edge, first
Convex edge is provided with screw, is fixed by the first sealing bolt 241 and temperature-control pressure-control device 2；The lower surface peace of first convex edge
Equipped with the first Graphite pad 242, the column outer wall below the first convex edge is provided with the low temperature resistant O-ring 243 of the first polyurethane, is formed
It is multi-stage sealed.
Further, the external diameter of the top cover of temperature-control pressure-control device upper end cover 24 so, makes temperature control control more than the diameter of column
After pressure device upper end cover 24 loads, column outside is by the low temperature resistant O-ring 243 of the first polyurethane and the tubular of temperature-control pressure-control device
Inner wall sealing, the convex edge lower section of the protrusion of top cover is sealed it with the top of temperature-control pressure-control device by the first Graphite pad 242,
Realize multi-stage sealed, effect is preferable.
Temperature-control pressure-control device upper end cover 24 is connected with high-pressure nitrogen bottle, and gas is applied to device inside using high-pressure nitrogen bottle
Pressure, so that further apply pressure to liquid nitrogen, when air pressure is more than the critical pressure of liquid nitrogen in device（3.3958MPa）, with
Temperature rises liquid nitrogen and will not gasify.
After using temperature-control pressure-control device regulation liquid nitrogen to preset temperature pressure, shale core is taken from rock core heater box
Go out, be positioned in freezing-thawing damage device；The second valve is opened, to nitrogen is filled with freezing-thawing damage device, reaches air pressure in device
To freeze thawing pressure, ensure that liquid nitrogen does not occur during being flowed into freezing-thawing damage device from temperature-control pressure-control device its object is to work as
Gasification；Temperature-control pressure-control device tapping valve is opened, according to law of connected vessels, liquid nitrogen flows into freezing-thawing damage device from temperature-control pressure-control device
Until stream oriented device liquid level is identical.
Liquid nitrogen temperature pressure stage, the first valve, the second valve, emptying valve, discharge opeing are adjusted using temperature-control pressure-control device
Valve is in closed mode, micro to open in emptying valve regulation temperature-control pressure-control device pressure extremely after the completion of regulation temperature, pressure
Freeze thawing pressure, closes atmospheric valve；Shale core is taken out from cabinet-type electric furnace and is discarded to freezing-thawing damage device, open the second valve
Door, air pressure in freezing-thawing damage device is promoted to the first valve is opened after freeze thawing pressure, closes total intake valve.
In addition, referring to the drawings 1 and 4,5 points of the freezing-thawing damage device that the present invention is mentioned is inside and outside two-layers, its internal layer is second
Deep cooling steel inner bag 52, outer layer is the second polyurethane adiabatic layer 51, and the second polyurethane adiabatic layer 51 is by freezing-thawing damage device upper end
In lid 54 is wrapped in, the second ultralow temperature temperature sensor 55, second is installed on the freezing-thawing damage device upper end cover 54 at top and is pressed
Force snesor 56, acoustic emission sensor 58, control pressure valve 53 and low temperature foil gauge wire 59.
Further, freezing-thawing damage device upper end cover 54 is made up of top cover and column, and the outer ring of top cover is provided with the second convex edge,
Second convex edge is provided with screw, is fixed by the second sealing bolt 541 and freezing-thawing damage device 5；The following table of second convex edge
Face is provided with the second Graphite pad 542, and the column outer wall below the second convex edge is provided with the low temperature resistant O-ring 543 of the second polyurethane,
Formed multi-stage sealed.
In addition, diameter of the external diameter of the top cover of freezing-thawing damage device upper end cover 54 more than column, structure and above-mentioned temperature control
Pressure control device upper end cover is similar to.
Furthermore, the two-way of four-way temperature and pressure digital display 3 respectively with the first ultralow temperature temperature of the top of temperature-control pressure-control device 2
Degree sensor 25, first pressure sensor 26 are connected；Another two-way respectively with the second ultralow temperature temperature of the top of freezing-thawing damage device 5
Sensor 55, second pressure sensor 56 are connected.
The top of above-mentioned high-pressure nitrogen bottle 4 is provided with pressure gauge 41, pressure-reducing valve 42 and total air intake valve 43, and and gases at high pressure
Pipeline 27 is connected.
A kind of experimental technique of liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision that the present invention is mentioned, specific steps are such as
Under：
(a), prepare rock core to be tested, shale core 6 is heated to preset temperature using cabinet-type electric furnace, check and confirm liquid nitrogen control
Temperature control presses each valve on freezing-thawing damage shale experimental provision and pipeline to be closed；
(b), open from supercharging liquid nitrogen container liquid feed valve 12, precooling carried out to device to a small amount of liquid nitrogen is filled in temperature-control pressure-control device 2,
Temperature-control pressure-control device atmospheric valve 28 is opened, is waited in complete discharge device and is closed atmospheric valve after nitrogen；
C (), shale freezing-thawing damage are tested
1. the liquid feed valve 12 from supercharging liquid nitrogen container 1 is opened, to liquid nitrogen is filled in temperature-control pressure-control device 2, liquid feed valve is closed；Beat
The pressure-reducing valve 42 of high-pressure nitrogen bottle 4 is driven, nitrogen pressure is adjusted to by default freeze thawing pressure according to pressure gauge；Open total air intake valve 43
With the first valve 271, nitrogen is filled with to temperature-control pressure-control device 2, when four-way temperature, pressure digital display 3 shows temperature-control pressure-control
After air pressure reaches freeze thawing pressure in device 2, now, freeze thawing pressure is more than the saturated vapour pressure of nitrogen at such a temperature, and its purpose exists
In ensuring that liquid nitrogen do not vaporize in heating process, nitrogen saturated vapour pressure at different temperatures is shown in accompanying drawing 5；Close the first valve
Door 271；Heating plate 23 is opened, liquid nitrogen is heated, when liquid nitrogen temperature is close to default freeze thawing temperature, close heating plate 23,
Liquid nitrogen is heated using heating plate waste heat；Micro opening atmospheric valve 28, air pressure is to jelly in slow regulation temperature-control pressure-control device
Melt pressure, the pressure that liquid nitrogen volumetric expansion is caused in elimination heating process rises；
2. shale core 6 is taken out from cabinet-type electric furnace, sticks low temperature resistant foil gauge 61 and be positioned in freezing-thawing damage device 5；Beat
The second valve 571 is opened, to nitrogen is filled with freezing-thawing damage device 5, after air pressure reaches freeze thawing pressure in freezing-thawing damage device, is closed
Total air intake valve 43 is closed, the first valve 271 is opened；Open temperature-control pressure-control device tapping valve 29, according to law of connected vessels, liquid nitrogen from
Temperature-control pressure-control device 2 flows into freezing-thawing damage device 5 until stream oriented device liquid level is identical；
D in (), shale frozen-thaw process, gas pressure in the real-time monitoring freezing-thawing damage device 5 of control pressure valve 53 eliminates liquid nitrogen
The pressure oscillation that vaporization is caused, it is ensured that freeze thawing pressure is fixed value；
After the completion of (e), shale frozen process experiment, the pressure release of atmospheric valve 28 of temperature-control pressure-control device is opened, take out shale core, tested
Finish.
Compared with prior art, its advantage is the present invention：
(1), experimental system is divided into two large divisions, liquid nitrogen temperature-control pressure-control and shale freeze thawing deterioration are carried out respectively, it is to avoid two parts
Between interfere, using heating plate and ultralow temperature temperature sensor accuracy controlling liquid nitrogen temperature, realize different cold shock temperature
Liquid nitrogen effect shale freezing-thawing damage experiment under degree；
(2), pressurizeed to liquid nitrogen using high-pressure nitrogen bottle, carry out the shale under different freeze thawing pressure and damage deterioration experiment, investigated and freeze
Melt the influence that pressure is damaged to the lower shale of liquid nitrogen effect；
(3), using cabinet-type electric furnace for rock core is heated, the temperature change in both direction is realized, investigates the identical temperature difference not equality of temperature
The degree influence that is damaged to shale of scope, actual response actual formation situation, for ultra-low temperature liquid nitrogen fracturing developing shale air lift
For the experimental result with actual directive significance；
(4), shale freeze thawing deterioration process is monitored in real time using two kinds of detection means of sound emission and foil gauge, is research page
Rock damage development process provides crucial experimental data；
(5), once can freeze thawing multiple rock cores, experiment rock core size is diameter 25mm, and 50mm high, experimental technique is simple, operation side
Just, experimental error is small.
The above, is only part preferred embodiment of the invention, and any those of ordinary skill in the art may profit
Equivalent technical scheme is changed or is revised as with the technical scheme of above-mentioned elaboration.Therefore, according to technology of the 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 (10)
1. a kind of liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision, it is characterized in that：Including supercharging liquid nitrogen container certainly（1）, temperature control
Pressure control device（2）, freezing-thawing damage device（5）, high-pressure nitrogen bottle（4）, data collecting system；Certainly the supercharging liquid nitrogen container（1）It is logical
Cross low temperature resistant metal pipe line（7）With temperature-control pressure-control device（2）It is connected, low temperature resistant metal pipe line（7）On liquid feed valve is installed（12）
With ultralow temperature flowmeter（11）, from supercharging liquid nitrogen container（1）Inside is equipped with ultra-low temperature liquid nitrogen；The high-pressure nitrogen bottle（4）By height
Calm the anger fluid line（27）Respectively with temperature-control pressure-control device（2）With freezing-thawing damage device（5）Upper end connects, high-pressure nitrogen bottle（4）It is interior
Equipped with high pressure nitrogen；The temperature-control pressure-control device（2）Top temperature-control pressure-control device upper end cover is installed（24）, temperature-control pressure-control dress
Put（2）Bottom pass through low temperature resistant metal pipe line（7）With freezing-thawing damage device（5）Bottom connection, temperature-control pressure-control device（2）Under
Portion exit is provided with tapping valve（29）；
The freezing-thawing damage device（5）Inside is provided with one or more shale core（6）, shale core（6）It is provided with
Low temperature foil gauge（61）, and by low temperature foil gauge（61）With the strain testing instrument of data collecting system（9）Connection, damages in freeze thawing
Hinder device（5）Top be provided with freezing-thawing damage device upper end cover（54）, bottom is provided with and low temperature resistant metal pipe line（7）What is connected goes out
Mouthful；
The data collecting system includes four-way temperature, pressure digital display（3）, acoustic emission detector（8）, strain testing
Instrument（9）And computer（10）, wherein, acoustic emission detector（8）With strain testing instrument（9）Monitoring Data is by computer（10）It is responsible for
Record.
2. liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision according to claim 1, it is characterized in that：The temperature control control
Pressure device（2）It is divided into inside and outside two-layer, its internal layer is the first deep cooling steel inner bag（22）, outer layer be the first polyurethane adiabatic layer（21）,
And first polyurethane adiabatic layer（21）By temperature-control pressure-control device upper end cover（24）In being wrapped in, temperature-control pressure-control device（2）Bottom
Heating plate is provided between inner bag and outer layer（23）, temperature-control pressure-control device（2）Top temperature-control pressure-control device upper end cover（24）Peace
Equipped with ultralow temperature temperature sensor（25）, pressure sensor（26）And atmospheric valve（28）.
3. liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision according to claim 1, it is characterized in that：The temperature control control
Pressure device upper end cover（24）It is made up of top cover and column, the outer ring of top cover is provided with the first convex edge, and the first convex edge is provided with screw, is led to
Cross the first sealing bolt（241）With temperature-control pressure-control device（2）It is fixed；The lower surface of first convex edge is provided with the first graphite pads
Piece（242）, the column outer wall below the first convex edge is provided with the low temperature resistant O-ring of the first polyurethane（243）, formed multi-stage sealed.
4. liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision according to claim 1, it is characterized in that：The freeze thawing is damaged
Hinder device（5）It is divided into inside and outside two-layer, its internal layer is the second deep cooling steel inner bag（52）, outer layer is the second polyurethane adiabatic layer（51）,
And second polyurethane adiabatic layer（51）By freezing-thawing damage device upper end cover（54）In being wrapped in, the freezing-thawing damage device upper end at top
Lid（54）On the second ultralow temperature temperature sensor is installed（55）, second pressure sensor（56）, acoustic emission sensor（58）, control
Pressing pressure valve（53）With low temperature foil gauge wire（59）.
5. liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision according to claim 1, it is characterized in that：The freeze thawing is damaged
Hinder device upper end cover（54）It is made up of top cover and column, the outer ring of top cover is provided with the second convex edge, and the second convex edge is provided with screw, is led to
Cross the second sealing bolt（541）With freezing-thawing damage device（5）It is fixed；The lower surface of second convex edge is provided with the second graphite pads
Piece（542）, the column outer wall below the second convex edge is provided with the low temperature resistant O-ring of the second polyurethane（543）, formed multi-stage sealed.
6. liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision according to claim 1, it is characterized in that：The four-way
Temperature and pressure digital display（3）Two-way respectively with temperature-control pressure-control device（2）First ultralow temperature temperature sensor of top（25）,
One pressure sensor（26）Connection；Another two-way respectively with freezing-thawing damage device（5）Second ultralow temperature temperature sensor of top
（55）, second pressure sensor（56）Connection.
7. liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision according to claim 1, it is characterized in that：The elevated pressure nitrogen
Gas cylinder（4）Top be provided with pressure gauge（41）, pressure-reducing valve（42）With total air intake valve（43）, and with gases at high pressure pipeline（27）Even
It is logical.
8. liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision according to claim 3, it is characterized in that：The temperature control control
Pressure device upper end cover（24）Top cover external diameter more than column diameter.
9. liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision according to claim 5, it is characterized in that：The freeze thawing is damaged
Hinder device upper end cover（54）Top cover external diameter more than column diameter.
10. a kind of experiment of liquid nitrogen temperature-control pressure-control freezing-thawing damage shale experimental provision as claimed in any one of claims 1-9 wherein
Method, it is characterized in that comprising the following steps that：
(a), prepare rock core to be tested, using cabinet-type electric furnace by shale core（6）Preset temperature is heated to, is checked and is confirmed liquid nitrogen
Each valve is closed on temperature-control pressure-control freezing-thawing damage shale experimental provision and pipeline；
(b), open from supercharging liquid nitrogen container liquid feed valve（12）, to temperature-control pressure-control device（2）The interior a small amount of liquid nitrogen of filling is carried out to device
Precooling, opens temperature-control pressure-control device atmospheric valve（28）, wait in complete discharge device and close atmospheric valve after nitrogen；
C (), shale freezing-thawing damage are tested
1. open from supercharging liquid nitrogen container（1）On liquid feed valve（12）, to temperature-control pressure-control device（2）Interior filling liquid nitrogen, closes feed liquor
Valve；Open high-pressure nitrogen bottle（4）Pressure-reducing valve（42）, nitrogen pressure is adjusted to by default freeze thawing pressure according to pressure gauge；Open total
Air intake valve（43）With the first valve（271）, to temperature-control pressure-control device（2）Nitrogen is filled with, when four-way temperature, pressure numeral is aobvious
Show device（3）Display temperature-control pressure-control device（2）After interior air pressure reaches freeze thawing pressure, now, freeze thawing pressure is more than nitrogen at such a temperature
Saturated vapour pressure, its object is to ensure that liquid nitrogen is not vaporized in heating process；Close the first valve（271）；Open
Heating plate（23）, liquid nitrogen is heated, when liquid nitrogen temperature is close to default freeze thawing temperature, close heating plate（23）, using plus
Hot plate waste heat is heated to liquid nitrogen；Micro opening atmospheric valve（28）, air pressure is to freeze thawing pressure in slow regulation temperature-control pressure-control device
Power, the pressure that liquid nitrogen volumetric expansion is caused in elimination heating process rises；
2. by shale core（6）Taken out from cabinet-type electric furnace, stick low temperature resistant foil gauge（61）It is positioned over freezing-thawing damage device（5）
It is interior；Open the second valve（571）, to freezing-thawing damage device（5）Nitrogen is inside filled with, when air pressure reaches freeze thawing in freezing-thawing damage device
After pressure, total air intake valve is closed（43）, open the first valve（271）；Open temperature-control pressure-control device tapping valve（29）, according to even
Logical device principle, liquid nitrogen is from temperature-control pressure-control device（2）Flow into freezing-thawing damage device（5）Until stream oriented device liquid level is identical；
In (d), shale frozen-thaw process, control pressure valve（53）Real-time monitoring freezing-thawing damage device（5）Interior gas pressure, eliminates
The pressure oscillation that liquid nitrogen vaporization is caused, it is ensured that freeze thawing pressure is fixed value；
After the completion of (e), shale frozen process experiment, the atmospheric valve of temperature-control pressure-control device is opened（28）Pressure release, takes out shale core, experiment
Finish.
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