CN114383978B - CO 2 Device and method for testing contact angle of coal-rock component of water-coal system - Google Patents
CO 2 Device and method for testing contact angle of coal-rock component of water-coal system Download PDFInfo
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- CN114383978B CN114383978B CN202111650671.9A CN202111650671A CN114383978B CN 114383978 B CN114383978 B CN 114383978B CN 202111650671 A CN202111650671 A CN 202111650671A CN 114383978 B CN114383978 B CN 114383978B
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- 239000003245 coal Substances 0.000 title claims abstract description 67
- 239000011435 rock Substances 0.000 title claims abstract description 33
- 238000012360 testing method Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002347 injection Methods 0.000 claims abstract description 38
- 239000007924 injection Substances 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000009423 ventilation Methods 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 238000005192 partition Methods 0.000 claims abstract description 11
- 238000012544 monitoring process Methods 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 20
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 238000010998 test method Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 description 8
- 239000003921 oil Substances 0.000 description 7
- 239000010724 circulating oil Substances 0.000 description 6
- 238000005498 polishing Methods 0.000 description 4
- 244000137852 Petrea volubilis Species 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000012625 in-situ measurement Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 230000009919 sequestration Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
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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
- G01N13/02—Investigating surface tension of liquids
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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
- G01N13/02—Investigating surface tension of liquids
- G01N2013/0208—Investigating surface tension of liquids by measuring contact angle
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P90/00—Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
- Y02P90/70—Combining sequestration of CO2 and exploitation of hydrocarbons by injecting CO2 or carbonated water in oil wells
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The invention discloses a CO 2 The water-coal system coal-rock component contact angle testing device and method, wherein the outside of the high-temperature high-pressure reaction cavity is wrapped with a temperature control system; the high-temperature high-pressure reaction cavity is sealed and separated into a left cavity and a right cavity by a lifting partition plate; a clamping frame for clamping the coal substrate is arranged in the right chamber, a perspective window corresponding to the clamping frame is arranged on the front side wall and the right side wall of the right chamber, and a camera facing the clamping frame is arranged on the outer side of the perspective window; the liquid injection system is communicated with the top of the left cavity; the ventilation system is communicated with the bottom of the left chamber; the ventilation system is used for providing CO 2 And/or CH 4 A gas; the pressure control valve path is connected between the left chamber and the right chamber and is used for realizing gas circulation of the left chamber and the right chamber; the air bubble pipeline is communicated with the left cavity and the right cavity, one end of the air bubble pipeline is positioned at the upper part of the left cavity, and the other end of the air bubble pipeline is positioned below the coal matrix and is used for expanding air bubbles to the bottom surface of the coal matrix; the temperature and pressure monitoring system is used for monitoring the air pressure of the left chamber and the air pressure and temperature of the right chamber.
Description
Technical Field
The invention relates to the technical field of wettability evaluation, in particular to a high-temperature high-pressure CO 2 -water-coal system coal-rock component contact angle testing device and method.
Background
Wettability refers to the ability of two mutually immiscible liquids to first wet a solid surface, i.e., the ability or tendency of a liquid to spread over a solid surface. Wetting phenomenon is very common in real life and scientific research. In CO 2 Wettability is an important surface phenomenon that affects mass transport and microscopic distribution of fluids in reservoirs during geological sequestration. The interfacial interactions, represented by wettability, determine the fluid distribution and behavior in the porous media.
The lubricity is generally expressed by the contact angle, and methods for measuring the contact angle include three main types of quantitative measurement, qualitative measurement and in-situ measurement. However, under high temperature and high pressure conditions, CO cannot be obtained directly by contact angle measurement 2 -water-coal system coal-rock component contact angle and cannot directly react CO in the system 2 Air wettability.
Therefore, how to provide a method for directly measuring CO under the condition of high temperature and high pressure by acquiring different coal and rock components 2 The contact angle testing device and method of the water-coal system are the problems to be solved by the person skilled in the art.
Disclosure of Invention
In view of this, the present invention provides a CO 2 The device and the method for testing the contact angle of the coal-rock component of the water-coal system aim at solving the technical problems.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
CO (carbon monoxide) 2 -a water-coal system coal-rock component contact angle testing device comprising:
a high-temperature high-pressure reaction chamber; a temperature control system is wrapped outside the high-temperature high-pressure reaction cavity; the high-temperature high-pressure reaction cavity is sealed and separated into a left cavity and a right cavity by a lifting partition plate; a clamping frame for clamping a coal substrate is arranged in the right chamber, a perspective window corresponding to the clamping frame is arranged on the front side wall and the right side wall of the right chamber, and a camera facing the clamping frame is arranged on the outer side of the perspective window;
a liquid injection system; the liquid injection system is positioned at the outer side of the high-temperature high-pressure reaction cavity and is communicated with the top of the left cavity;
a ventilation system; the ventilation system is positioned outside the high-temperature high-pressure reaction cavity and is communicated with the bottom of the left cavity; the ventilation system is used for providing CO 2 And/or CH 4 A gas;
a pressure control valve path; the pressure control valve path is positioned at the outer side of the high-temperature high-pressure reaction cavity, connected between the left cavity and the right cavity and used for realizing gas circulation from the left cavity to the right cavity;
a bubble line; the air bubble pipeline is communicated with the left cavity and the right cavity, one end of the air bubble pipeline is positioned at the upper part of the left cavity, and the other end of the air bubble pipeline is positioned below the coal substrate and is used for expanding air bubbles to the bottom surface of the coal substrate;
a temperature and pressure monitoring system; the temperature and pressure monitoring system is used for monitoring the air pressure of the left chamber and the air pressure and temperature of the right chamber.
Through the technical scheme, the device provided by the invention can be used for adjusting the position of the camera outside the cavity to be opposite to CO under the conditions of high temperature and high pressure 2 The contact position of the bubble and the coal is adjusted, and the laser beam is irradiated to the contact center position of the bubble; the whole process is video recorded by a camera outside the chamber through a transparent high-pressure glass window, an image is extracted to carry out contact angle measurement calculation, and the method directly obtains CO through contact angle measurement 2 -water-coal system coal-rock component contact angle and capable of directly reacting CO in the system 2 Air wettability.
Preferably, one of the above-mentioned COs 2 In the water-coal system coal-rock component contact angle testing device, the temperature control system comprises a double-layer shell formed on the outer side wall of the high-temperature high-pressure reaction cavity, and the space between the double-layer shellsThe gap cavity is filled with oil bath liquid; the double-layer shell is characterized in that the outer side wall of the double-layer shell is provided with a circulating oil inlet and a circulating oil return port, an oil circulating pipeline positioned at the outer side of the double-layer shell is connected between the circulating oil inlet and the circulating oil return port, and a circulating pump and a constant-temperature heating device are arranged on the oil circulating pipeline. The circulation oil inlet is located right side wall upper portion of right cavity, the circulation oil return mouth is located left side wall lower part of left cavity can make fluid heating more even.
Preferably, one of the above-mentioned COs 2 In the water-coal system coal-rock component contact angle testing device, the clamping frame is fixed at the middle lower part of the right cavity through a bracket, the clamping frame is a square pipe with a rectangular cross section, the axial direction of the square pipe is horizontally arranged and is vertical to the front side wall of the right cavity, the bottom surface of the square pipe is axially provided with a notch penetrating through two ends, the coal substrate is placed in the square pipe, and air bubbles bulged out of the air bubble pipeline are contacted with the bottom surface of the coal substrate through the notch; and graduated scales are arranged on the top surface of the square tube towards the two edges of the two cameras. The scale of the scale can enable the camera to carry out plane positioning on the position of the contact angle of the coal sample through the photographed pictures in two directions.
Preferably, one of the above-mentioned COs 2 -in a water-coal system coal-rock component contact angle testing device, the liquid injection system comprises a water tank which is communicated with the top wall of the left chamber through a liquid injection pipe; a high-pressure injection pump and an injection valve are sequentially arranged on the injection pipe from the water tank to the left cavity; the left chamber is also provided with a stirrer; the stirrer comprises a stirring motor and a stirring shaft; the stirring motor is fixed on the outer top wall of the left cavity, the stirring shaft is vertically arranged inside the left cavity, the top end of the stirring shaft is connected with a power output shaft of the stirring motor, and stirring blades are uniformly fixed on the stirring shaft.
Preferably, one of the above-mentioned COs 2 -in a water-coal system coal-rock component contact angle testing device, the ventilation system comprises CO 2 Gas cylinder and CH 4 A gas cylinder; the CO 2 Gas cylinder and said CH 4 The gas cylinders are communicated with the bottom wall of the left cavity through a ventilation pipeline after being connected in parallel; the vent pipeline is connected with the CO 2 Gas cylinder and said CH 4 A booster pump, a pressure reducing valve, a constant pressure constant speed pump and an electric regulating valve are sequentially arranged on the gas cylinder towards the left chamber; the booster pump is connected with an air compressor; the CO 2 Gas cylinder and said CH 4 And branch control valves are respectively arranged on the parallel branches of the gas cylinders.
Preferably, one of the above-mentioned COs 2 -in the water-coal system coal-rock component contact angle testing device, the pressure control valve circuit comprises a pressure control pipeline connected to the top walls of the left chamber and the right chamber; the pressure control pipeline is provided with a one-way valve, and the one-way valve can only enable gas to flow from the left chamber to the right chamber; the pressure control pipeline between the one-way valve and the right chamber is provided with two parallel branches, and the two branches are respectively provided with a first pressure relief valve and a first emptying valve.
Preferably, one of the above-mentioned COs 2 In the water-coal system coal-rock component contact angle testing device, the left chamber is also connected with a vacuum system; the vacuum system comprises a vacuum pump, the vacuum pump is communicated with the left side wall of the left cavity through a vacuum pipeline, and a vacuum pump control valve is arranged on the vacuum pipeline; the vacuum pump control valve and the vacuum pipeline between the left cavity are provided with two parallel branches, and the two branches are respectively provided with a second pressure relief valve and a second emptying valve.
Preferably, one of the above-mentioned COs 2 -in a water-coal system coal-rock component contact angle testing device, the bubble line comprises a first line, a second line and a connecting hose; the first pipeline is vertically arranged in the left cavity, the top end of the first pipeline is positioned at the upper part of the left cavity, and the bottom end of the first pipeline penetrates out of the left cavity; the second pipeline is vertically arranged in the right cavity, the top end of the second pipeline is provided with an injection needle towards the bottom surface of the coal matrix, and the bottom end of the second pipeline penetrates out of the right cavity; the connecting hose is communicated with the bottom ends of the first pipeline and the second pipeline, and an electric needle valve is arranged on the connecting hose.
Preferably, one of the above-mentioned COs 2 In the water-coal system coal-rock component contact angle testing device, the temperature and pressure monitoring system comprises a first pressure sensor arranged on the top wall of the left chamber, a second pressure sensor arranged on the top wall of the right chamber, and a temperature sensor arranged on the right side wall of the right chamber.
Preferably, one of the above-mentioned COs 2 In the water-coal system coal-rock component contact angle testing device, the lifting partition plate is controlled to lift by a nut valve arranged on the outer top wall of the high-temperature high-pressure reaction cavity. The structural principle of the nut valve is the same as that of the ball screw, and the lifting partition plate is driven to lift by the rotation of the nut.
Preferably, one of the above-mentioned COs 2 In the water-coal system coal-rock component contact angle test device, the lower part of the right side wall of the right chamber is provided with a discharge pipeline, and a discharge control valve is arranged on the discharge pipeline.
Preferably, one of the above-mentioned COs 2 In the water-coal system coal-rock group contact angle testing device, the first pressure sensor, the second pressure sensor, the temperature sensor and the electric needle valve are electrically connected with a signal receiver, the signal receiver is electrically connected with a control terminal, and the control terminal can be a computer.
The invention also provides a CO 2 -water-coal system coal-rock composition contact angle test method using one of the above-mentioned CO 2 -water-coal system coal-rock component contact angle testing device for CO under high temperature and high pressure state 2 -water-coal system coal-rock component contact angle detection.
As can be seen from the technical scheme, compared with the prior art, the invention discloses a CO 2 The device and the method provided by the invention can directly obtain CO through contact angle measurement 2 -water-coal system coal-rock component contact angle and capable of directly reacting CO in the system 2 Air wettability.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a testing device according to the present invention;
FIG. 2 is a right side view of the high temperature and high pressure reaction chamber provided by the invention;
FIG. 3 is a front view of the clamping frame provided by the invention;
FIG. 4 is a right side view of the clamping frame provided by the invention;
fig. 5 is a top view of the clamping frame provided by the invention.
Wherein:
1-a high-temperature high-pressure reaction chamber; 2-lifting a partition plate; 3-left chamber; 4-right chamber; 5-clamping frames; 6-perspective window; 7-a video camera; 8-a double-layer shell; 9-oil bath; 10-a circulating oil inlet; 11-circulating oil return port; 12-an oil circulation pipeline; 13-a circulation pump; 14-a constant temperature heating device; 15-a graduated scale; 16-a water tank; 17-a liquid injection pipe; 18-a high pressure injection pump; 19-a liquid injection valve; 20-a stirring motor; 21-a stirring shaft; 22-CO 2 A gas cylinder; 23-CH 4 A gas cylinder; 24-a vent line; 25-booster pump; 26-a pressure reducing valve; 27-constant pressure constant speed pump; 28-an electric regulating valve; 29-an air compressor; 30-branch control valve; 31-a pressure control pipeline; 32-a one-way valve; 33-a first pressure relief valve; 34-a first drain valve; 35-a vacuum pump; 36-vacuum line; 37-a vacuum pump control valve; 38-a second pressure relief valve; 39-a second drain valve; 40-a first pipeline; 41-a second line; 42-connecting a hose; 43-an injection needle; 44-electric needle valve; 45-a first pressure sensor; 46-a second pressure sensor; 47-temperature sensor; 48-nut valve; 49-a discharge conduit; 50-a discharge control valve; 51-signal receiver; 52-a control terminal; 53-coal matrix.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1 to 5, the embodiment of the invention discloses a CO 2 The water-coal system coal-rock component contact angle testing method specifically comprises the following steps:
(1) Firstly, selecting coal blocks, cutting coal slices from the large-sized coal blocks, and cutting the coal samples into square slices, wherein the sizes of the square slices are about 21mm multiplied by 4mm.
(2) Polishing and roughing the cut coal sample by using 220-320 mesh silicon carbide sand paper to remove small scratches; then sequentially adopting 400-10000 mesh silicon carbide sand paper to conduct fine grinding and wet polishing.
(3) And (3) drying the sample at room temperature for at least 72 hours, and measuring the surface roughness by using an atomic force microscope or a surface roughness measuring instrument after cleaning the surface to obtain a roughness Ra (arithmetic average roughness) value.
(4) When the Ra value is smaller than 0.1 mu m, the surface polishing of the sample is qualified, and the sample can be measured by equipment; if the Ra value is greater than 0.1 μm, further refining and polishing are required.
(5) The coal substrate 53 is clamped and fixed on the clamping frame 5 in the right chamber 4. The holder 5 is positioned in a field of view that is viewable through the see-through window 6. (see-through windows are provided 2, one on the right side as viewed in FIG. 1 and one on the front side perpendicular to the paper of FIG. 1); the right and front view of the holder 5 is shown in fig. 1. A graduated scale 15 is arranged above the clamping frame 5 of the right view and the front view, and the position of the contact angle of the coal sample can be positioned in a plane by taking pictures in two directions.
(6) The constant temperature heating device 14 and the circulating pump 13 are turned on, the heat lamp and the light source are turned on, and the stable temperature is set at a set temperature value.
(7) The check valve 32 is opened to ensure that the left chamber 3 and the right chamber 4 are communicated, all valves except the check valve 32 are closed, the nut valve 48 is closed, the lifting partition plate 2 is tightly closed, and the air tightness of the device is ensured to be good.
(8) The vacuum pump 35 and the vacuum pump control valve 37 are opened, air in the high-temperature high-pressure reaction chamber 1 is discharged, and the vacuum pump 35 and the vacuum pump control valve 37 are closed after the air is discharged.
(9) The filling valve 19 is opened, the process water in the water tank 16 is filled into the left chamber 3 through the filling pipe 17 to the first water line at the upper part of fig. 1 by the high pressure filling pump 18, and the filling is stopped and the filling valve 19 is closed when the height is about five minutes of the water tank 16.
(10) The check valve 32 is kept in a closed state. The electric control valve 28 was opened, and the gas (CO) was injected through the booster pump 25 and the high-precision constant-pressure constant-speed pump 27 (precision 0.01 MPa) 2 Or CH (CH) 2 ) The method comprises the steps of carrying out a first treatment on the surface of the Gas (CO) 2 ) During the injection process, the electric control stirrer is turned on to stir the liquid in the left chamber 3 so as to promote CO 2 And H 2 The dissolution balance of O; at this time, CO in the left chamber 3 2 Will be partially dissolved in water, the upper part of which is CO 2 The lower part of the gas layer is towards saturated CO 2 Is a water layer of (2); the water level in the left chamber 3 is lower than the inlet of the first pipe 40 in the left chamber 3.
(11) The injection process obtains the pressure value in the cavity through the pressure sensor, and when a fixed pressure increment value is set (for example, the pressure interval is set to be 2 MPa), the one-way valve 32 is opened at intervals, so that the gas above the first water line of the left cavity 3 intermittently flows into the right cavity 4; the right chamber 4 is gas and the pressure gradually increases.
(12) The pressure in the chamber is gradually increased to a set experimental pressure value (the pressure value is obtained by 2 pressure sensors on the left and right chambers), the booster pump 25 and the electric control valve 28 are closed, and the injection of gas is stopped.
(13) The electronically controlled stirrer was turned off and left stationary for 5 hours, CO was established in the left chamber 3 2 And H 2 The dissolution balance and the pressure balance of O. The process check valve 32 is in an open state. At this time, the left and right chamber pressures tend to be the same (the left chamber 3 is measured as the upper air pressure, and the right chamber 4 is measured as the whole chamber air pressure), and the set pressure value is reached stably at the most.
(14) If the pressure in the left and right chambers is carelessly greater than the set pressure value (monitored by 2 high-precision pressure sensors of the left and right chambers), the pressure can be released (high-precision electric control valve is selected) to the set pressure respectively through 2 automatic pressure relief valves communicated with the left and right chambers respectively (when releasing, the check valve 32 is kept open, and one pressure relief valve can be opened); if the pressure is too low, repeating the steps 14-15.
(15) Rotating the nut valve 48 counterclockwise, lifting the lifting partition plate 2 by about 1cm, allowing water to slowly flow from the lower part of the left chamber 3 into the right chamber 4 along the bottom lifting position, and simultaneously keeping the check valve 32 open, so that supercritical CO in the right chamber 4 is obtained 2 Into the left chamber 3 (forming an upper gas flow cycle and a lower water flow cycle), when the two chamber levels are at the same level (where the level is at a level higher than the level of the coal matrix 53 in the right chamber 4 in the second water line in the middle of fig. 1), the device is stationary for about 1 hour; at the moment, the two chambers complete the balance of air pressure and density, and the CO in the water is saturated 2 CO in gas and coal 2 The gas adsorption is saturated.
(16) The nut valve 48 is rotated clockwise to tightly close the lifting partition plate 2; and closes the check valve 32. At this time, the water level in the left chamber 3 is lower than the inlet of the first pipe 40 in the left chamber 3; the left and right chambers are not in communication.
(17) The pressure of the constant pressure constant speed pump 27 is increased by 0.01Mpa based on the set pressure, the electric control valve 28 is opened, and the gas (CO) is injected into the left chamber 3 again 2 ) The method comprises the steps of carrying out a first treatment on the surface of the Under the pressure effect of 0.01MPa of pressurization, the air pressure in the left chamber 3 is increased (the pressure of the left chamber 3 is set to be 0.01MPa, the pressure of the right chamber 4 is set to be 0.01MPa, and the pressure difference between the left chamber and the right chamber is 0.01 MPa); opening the electric needle valve 44, the left chamber 3 is filled with CO 2 Gas will enter the right chamber 4 (after balancing the left and right chamber conditions) through the tubing via the injection needle 43. Control of CO by controlling the motorized needle valve 44 and the injection needle 43 2 The bubbles float upward in the form of bubbles.
(18) The injection needle 43 is movable up and down, the outer wall of the injection needle is fixed on the bin wall, and the internal injection device can realize stepless up and down movement; when CO 2 When the syringe needle is stuck, the syringe needle can be pulled down to lead CO 2 The bubbles are separated from the floating.
(19) After the first measurement of the beam, the position of the coal substrate 53 in the holder 5 is moved and the next station test is started.
(20)CO 2 When the air bubble is extruded out of the needle head, the positions of the right camera and the front camera outside the cavity are adjusted to be opposite to the contact position of the air bubble and the coal, and the laser beam is adjusted to irradiate to the contact center position of the air bubble; the whole process is that a right camera and a front camera outside the cavity record video through a transparent high-pressure glass window, and an image is extracted to perform contact angle measurement calculation.
(21) Contact angle calculation: the static contact angle was calculated by young's equation from photographs recorded immediately after contact of the bubbles with the coal substrate surface and stable equilibrium. The dynamic contact angle was then further calculated by young's equation using photographs taken during the movement of the bubbles.
(22) Taking out the sample, and drying at normal temperature; positioning CO by right camera and front camera shooting picture and holder 5 coordinate system 2 Contact a specific location of the coal-based surface. And marking and numbering each measuring point on the surface of the coal matrix.
(23) And (3) placing the sample under a microscopic densitometer, observing the microscopic components according to the standard, and obtaining the microscopic component information of each measuring point. Further, scanning electron microscopy can be used for surface observation of the test position.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. CO (carbon monoxide) 2 -water-coal system coal-rock component contact angle testing device, characterized by comprising:
a high-temperature high-pressure reaction chamber (1); a temperature control system is wrapped outside the high-temperature high-pressure reaction cavity (1); the high-temperature high-pressure reaction cavity (1) is hermetically separated into a left cavity (3) and a right cavity (4) by a lifting partition board (2); a clamping frame (5) for clamping a coal substrate (53) is arranged in the right chamber (4), a perspective window (6) corresponding to the clamping frame (5) is arranged on the front side wall and the right side wall of the right chamber (4), and a camera (7) facing the clamping frame (5) is arranged outside the perspective window (6);
a liquid injection system; the liquid injection system is positioned outside the high-temperature high-pressure reaction cavity (1) and is communicated with the top of the left cavity (3);
a ventilation system; the ventilation system is positioned outside the high-temperature high-pressure reaction cavity (1) and is communicated with the bottom of the left cavity (3); the ventilation system is used for providing CO 2 And/or CH 4 A gas;
a pressure control valve path; the pressure control valve path is positioned outside the high-temperature high-pressure reaction cavity (1) and connected between the left cavity (3) and the right cavity (4) and is used for realizing gas circulation from the left cavity (3) to the right cavity (4);
a bubble line; the air bubble pipeline is communicated with the left cavity (3) and the right cavity (4), one end of the air bubble pipeline is positioned at the upper part of the left cavity (3), and the other end of the air bubble pipeline is positioned below the coal matrix (53) and is used for expanding air bubbles to the bottom surface of the coal matrix (53);
a temperature and pressure monitoring system; the temperature and pressure monitoring system is used for monitoring the air pressure of the left chamber (3) and the air pressure and temperature of the right chamber (4);
the liquid injection system comprises a water tank (16), and the water tank (16) is communicated with the top wall of the left cavity (3) through a liquid injection pipe (17); a high-pressure injection pump (18) and an injection valve (19) are sequentially arranged on the injection pipe (17) from the water tank (16) to the left cavity (3); the left chamber (3) is also provided with a stirrer; the stirrer comprises a stirring motor (20) and a stirring shaft (21); the stirring motor (20) is fixed on the outer top wall of the left cavity (3), the stirring shaft (21) is vertically arranged inside the left cavity (3), the top end of the stirring shaft is connected with a power output shaft of the stirring motor (20), and stirring blades are uniformly fixed on the stirring shaft (21);
the ventilation system includes CO 2 Gas cylinder (22) and CH 4 A gas cylinder (23); the CO 2 Gas cylinder (22) and CH 4 The gas cylinders (23) are connected in parallel and then communicated with the bottom wall of the left chamber (3) through a ventilation pipeline (24); the CO is arranged on the ventilation pipeline (24) 2 Gas cylinder (22) and CH 4 A booster pump (25), a pressure reducing valve (26), a constant-pressure constant-speed pump (27) and an electric regulating valve (28) are sequentially arranged on the gas cylinder (23) towards the left chamber (3); the booster pump (25) is connected with an air compressor (29); the CO 2 Gas cylinder (22) and CH 4 Branch control valves (30) are respectively arranged on parallel branches of the gas cylinders (23);
the pressure control valve path comprises a pressure control pipeline (31) connected to the top walls of the left chamber (3) and the right chamber (4); a one-way valve (32) is arranged on the pressure control pipeline (31), and the one-way valve (32) can only enable gas to flow from the left chamber (3) to the right chamber (4); the pressure control pipeline (31) between the one-way valve (32) and the right chamber (4) is provided with two parallel branches, and a first pressure relief valve (33) and a first emptying valve (34) are respectively arranged on the two branches;
the bubble pipeline comprises a first pipeline (40), a second pipeline (41) and a connecting hose (42); the first pipeline (40) is vertically arranged in the left chamber (3), the top end of the first pipeline is positioned at the upper part of the left chamber (3), and the bottom end of the first pipeline penetrates out of the left chamber (3); the second pipeline (41) is vertically arranged in the right chamber (4), an injection needle (43) facing the bottom surface of the coal matrix (53) is arranged at the top end, and the bottom end penetrates out of the right chamber (4); the connecting hose (42) is communicated with the bottom ends of the first pipeline (40) and the second pipeline (41), and an electric needle valve (44) is arranged on the connecting hose (42);
opening a liquid injection valve (19), injecting the experimental water in the water tank (16) into a first water line of the left cavity (3) through a liquid injection pipe (17) by a high-pressure injection pump (18), stopping injection when the height is five minutes of the water tank (16), and closing the liquid injection valve (19);
maintaining the one-way valve (32) in a closed state; the electric regulating valve (28) is opened, and CO is injected through the booster pump (25) and the constant-pressure constant-speed pump (27) 2 Or CH (CH) 4 ；CO 2 During the injection process, the stirrer is turned on to stir the liquid in the left chamber (3) so as to promote CO 2 And H 2 The dissolution balance of O; at this time, CO in the left chamber (3) 2 Will be partially dissolved in water, the upper part of which is CO 2 The lower part of the gas layer is towards saturated CO 2 Is a water layer of (2); the water level in the left chamber (3) is lower than the inlet of a first pipeline (40) in the left chamber (3);
the injection process obtains the pressure value in the cavity through the pressure sensor, and when a fixed pressure increment value is set, the one-way valve (32) is opened at intervals, so that the gas above the first water line of the left cavity (3) intermittently flows into the right cavity (4); the right chamber (4) is gas, and the pressure is gradually increased;
gradually increasing the pressure in the cavity to a set experimental pressure value, closing the booster pump (25) and the electric regulating valve (28), and stopping injecting gas;
the stirrer was turned off and allowed to stand for 5 hours to establish CO in the left chamber (3) 2 And H 2 The dissolution balance and the pressure balance of O; the process check valve (32) is in an open state, at the moment, the pressures of the left chamber (3) and the right chamber (4) tend to be the same, and finally the pressure value is stably reached;
lifting the lifting partition board (2) by 1cm to enable water to flow from the left chamber(3) The lower part flows into the right chamber (4) along the bottom lifting position, and simultaneously the one-way valve (32) is kept to be opened, so that the supercritical CO in the right chamber (4) is realized 2 Flowing into the left chamber (3), and standing for 1 hour when the horizontal planes of the left chamber (3) and the right chamber (4) are at the same height; at the moment, the left chamber (3) and the right chamber (4) finish the air pressure and density balance, and the CO in the water is saturated 2 CO in gas and coal 2 Gas adsorption saturation;
closing the lifting partition board (2); and closing the one-way valve (32); at the moment, the water level in the left chamber (3) is lower than the inlet of the first pipeline (40) in the left chamber (3); the left chamber (3) and the right chamber (4) are not communicated;
the pressure of the constant-pressure constant-speed pump (27) is increased by 0.01Mpa based on the set pressure, an electric regulating valve (28) is opened, and CO is injected into the left chamber (3) again 2 The method comprises the steps of carrying out a first treatment on the surface of the Under the pressure effect of pressurizing 0.01MPa, the air pressure in the left chamber (3) is increased; opening the electric needle valve (44) to allow CO in the left chamber (3) 2 The gas enters the right chamber (4) through the pipeline and the injection needle (43); control of CO by controlling an electric needle valve (44) and an injection needle (43) 2 The bubbles float upward in the form of bubbles.
2. A CO according to claim 1 2 -a water-coal system coal-rock component contact angle testing device, which is characterized in that the temperature control system comprises a double-layer shell (8) formed on the outer side wall of the high-temperature high-pressure reaction cavity (1), and an oil bath liquid (9) is filled in a clearance cavity of the double-layer shell (8); the double-layer shell (8) lateral wall has circulation oil inlet (10) and circulation oil return opening (11), circulation oil inlet (10) with be connected with between circulation oil return opening (11) and be located fluid circulation pipeline (12) in the outside of double-layer shell (8), install circulating pump (13) and constant temperature heating device (14) on fluid circulation pipeline (12).
3. A CO according to claim 1 2 Water-coal system coal-rock composition contact angle test deviceThe device is characterized in that the clamping frame (5) is fixed at the middle lower part of the right cavity (4) through a bracket, the clamping frame (5) is a square tube with a rectangular cross section, the axial direction of the square tube is horizontally arranged and is perpendicular to the front side wall of the right cavity (4), the bottom surface of the square tube is axially provided with a notch penetrating through two ends, the coal substrate (53) is placed in the square tube, and air bubbles bulged out of the air bubble pipeline are contacted with the bottom surface of the coal substrate (53) through the notch; and graduated scales (15) are arranged on the top surface of the square tube towards the two edges of the two cameras (7).
4. A CO according to claim 1 2 -water-coal system coal-rock component contact angle testing device, characterized in that the left chamber (3) is also connected with a vacuum system; the vacuum system comprises a vacuum pump (35), the vacuum pump (35) is communicated with the left side wall of the left cavity (3) through a vacuum pipeline (36), and a vacuum pump control valve (37) is arranged on the vacuum pipeline (36); the vacuum pipeline (36) between the vacuum pump control valve (37) and the left chamber (3) is provided with two parallel branches, and a second pressure relief valve (38) and a second emptying valve (39) are respectively arranged on the two branches.
5. A CO according to claim 1 2 -water-coal system coal-rock composition contact angle testing device, characterized in that the temperature and pressure monitoring system comprises a first pressure sensor (45) mounted on the top wall of the left chamber (3), and a second pressure sensor (46) mounted on the top wall of the right chamber (4), and a temperature sensor (47) mounted on the right side wall of the right chamber (4).
6. CO (carbon monoxide) 2 -water-coal system coal-rock composition contact angle test method characterized by using a CO according to any one of claims 1-5 2 -water-coal system coal-rock component contact angle testing device for CO under high temperature and high pressure state 2 Water-coal system coal-rock group contact angle realizing detectionAnd (5) measuring.
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