CN114383978A - CO2Testing device and method for coal-rock component contact angle of water-coal system - Google Patents
CO2Testing device and method for coal-rock component contact angle of water-coal system Download PDFInfo
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- CN114383978A CN114383978A CN202111650671.9A CN202111650671A CN114383978A CN 114383978 A CN114383978 A CN 114383978A CN 202111650671 A CN202111650671 A CN 202111650671A CN 114383978 A CN114383978 A CN 114383978A
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- 239000003245 coal Substances 0.000 title claims abstract description 81
- 239000011435 rock Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000002347 injection Methods 0.000 claims abstract description 35
- 239000007924 injection Substances 0.000 claims abstract description 35
- 238000012360 testing method Methods 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 239000011159 matrix material Substances 0.000 claims abstract description 19
- 238000012544 monitoring process Methods 0.000 claims abstract description 10
- 238000009423 ventilation Methods 0.000 claims abstract description 6
- 238000005273 aeration Methods 0.000 claims abstract description 4
- 238000003825 pressing Methods 0.000 claims abstract description 3
- 238000007664 blowing Methods 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 16
- 239000010724 circulating oil Substances 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 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
- 230000000149 penetrating effect Effects 0.000 claims description 2
- 238000013022 venting Methods 0.000 claims 1
- 238000005259 measurement Methods 0.000 description 5
- 238000005192 partition Methods 0.000 description 4
- 238000009736 wetting Methods 0.000 description 4
- 238000005498 polishing Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 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
- 239000000243 solution Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000009919 sequestration Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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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
-
- 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
Abstract
The invention discloses CO2The testing device and method for the contact angle of the coal and rock component of the water-coal system are characterized in that a temperature control system is wrapped outside a high-temperature high-pressure reaction cavity; the high-temperature high-pressure reaction cavity is hermetically divided into a left cavity and a right cavity by a lifting clapboard; a clamping frame used for clamping the coal matrix 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 chamber; the ventilation system is communicated with the bottom of the left chamber; aeration system for providing CO2And/or CH4A gas; the pressure control valve circuit is connected between the left chamber and the right chamber and is used for realizing the gas circulation of the left chamber to 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 blowing air bubbles to the bottom surface of the coal matrix; the warm-pressing 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 high-temperature high-pressure CO2A water-coal system coal-rock component contact angle testing device and a method.
Background
Wettability refers to the presence of two immiscible liquids, the ability of a liquid to first wet a solid surface, i.e., the ability or propensity of a liquid to spread on a solid surface. The phenomenon of wetting is very common in real life as well as in scientific research. In CO2Wettability is an important surface phenomenon affecting the transport of materials and the micro-distribution of fluids in reservoirs during geological sequestration. Interfacial interactions, represented by wettability, determine fluid distribution and behavior in porous media.
The lubricity is generally expressed by contact angle, and methods for measuring contact angle include three major categories, namely quantitative determination, qualitative determination and in-situ determination. However, under the conditions of high temperature and high pressure, CO can not be directly obtained through contact angle measurement2Water-coal system coal-rock component contact angle and not capable of directly reacting CO in the system2Gas wetting property.
Therefore, how to provide a method for directly measuring CO under high-temperature and high-pressure conditions by obtaining different coal rock components2The contact angle testing device and method of the water-coal system are problems which need to be solved by the technical personnel in the field.
Disclosure of Invention
In view of the above, the present invention provides a CO2A water-coal system coal-rock component contact angle testing device and a method, aiming at solving the technical problems.
In order to achieve the purpose, the 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; the outer side of the high-temperature high-pressure reaction cavity is wrapped with a temperature control system; the high-temperature high-pressure reaction cavity is hermetically divided into a left cavity and a right cavity by a lifting clapboard; a clamping frame used for clamping the coal matrix 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 erected on the outer side of the perspective window;
a liquid injection system; the liquid injection system is positioned outside 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 aeration system is used for providing CO2And/or CH4A gas;
a pressure control valve circuit; the pressure control valve circuit is positioned outside the high-temperature high-pressure reaction cavity, is connected between the left chamber and the right chamber, and is used for realizing gas circulation from the left chamber to the right chamber;
a bubble pipe line; the bubble pipeline is communicated with the left chamber and the right chamber, one end of the bubble pipeline is positioned at the upper part of the left chamber, and the other end of the bubble pipeline is positioned below the coal matrix and is used for bubbling bubbles to the bottom surface of the coal matrix;
a warm pressure monitoring system; the warm-pressing 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 enable the camera to be opposite to CO by adjusting the position of the camera outside the cavity under the conditions of high temperature and high pressure2Adjusting the contact position of the bubbles and the coal, and adjusting the laser beam to irradiate the contact center position of the bubbles; in the whole process, a video is recorded by a camera outside the chamber through a transparent high-pressure glass window, and an image is extracted for measuring and calculating the contact angle2Water-coal system coal-rock component contact angle and capable of directly reacting CO in the system2Gas wetting property.
Preferably, in one of the above-mentioned COs2In the coal rock component contact angle testing device of the water-coal system, the temperature control system comprises a double-layer shell formed on the outer side wall of the high-temperature high-pressure reaction cavityOil bath liquid is filled in the gap cavity of the double-layer shell; 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 located on 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 installed on the oil circulating pipeline. The oil circulation inlet is located on the upper portion of the right side wall of the right cavity, and the oil circulation return inlet is located on the lower portion of the left side wall of the left cavity, so that oil can be heated more uniformly.
Preferably, in one of the above-mentioned COs2In the coal-rock component contact angle testing device of the water-coal system, the clamping frame is fixed at the middle lower part of the right cavity through a support, the clamping frame 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, notches penetrating through two ends are axially formed in the bottom surface of the square tube, the coal matrix is placed in the square tube, and bubbles blown out from the bubble pipeline are in contact with the bottom surface of the coal matrix through the notches; the square tube top surface faces two the two edges of the camera are provided with graduated scales. The scale scales of the graduated scale can enable the camera to carry out plane positioning on the position measured by the coal sample contact angle through the shot pictures in two directions.
Preferably, in one of the above-mentioned COs2In the coal-rock component contact angle testing device of the water-coal system, 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 chamber; 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 chamber, the stirring shaft is vertically arranged inside the left chamber, the top end of the stirring shaft is connected with the power output shaft of the stirring motor, and stirring blades are uniformly fixed on the stirring shaft.
Preferably, in one of the above-mentioned COs2-in a water-coal system coal rock component contact angle testing device, the aeration system comprises CO2Gas cylinder and CH4A gas cylinder; the CO is2Gas cylinder and said CH4The gas cylinders are connected in parallel and then communicated with the bottom wall of the left chamber through a vent pipeline; the CO is arranged on the ventilation pipeline2Gas cylinder and said CH4A booster pump, a pressure reducing valve, a constant-pressure constant-speed pump and an electric regulating valve are sequentially arranged on the gas cylinder in the direction of the left chamber; the booster pump is connected with an air compressor; the CO is2Gas cylinder and said CH4Branch control valves are respectively arranged on the parallel branches of the gas cylinder.
Preferably, in one of the above-mentioned COs2In the coal-rock component contact angle testing device of the water-coal system, the pressure control valve circuit comprises a pressure control circuit 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 only enables gas to flow from the left chamber to the right chamber; the control pressure 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 release valve and a first emptying valve.
Preferably, in one of the above-mentioned COs2In the device for testing the contact angle of the coal rock component of the water-coal system, 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 installed on the vacuum pipeline; and two parallel branches are arranged on the vacuum pipeline between the vacuum pump control valve and the left chamber, and a second pressure release valve and a second evacuation valve are respectively arranged on the two branches.
Preferably, in one of the above-mentioned COs2-in a water-coal system coal rock component contact angle testing device, the bubble pipeline comprises a first pipeline, a second pipeline and a connecting hose; the first pipeline is vertically arranged in the left chamber, the top end of the first pipeline is positioned at the upper part of the left chamber, and the bottom end of the first pipeline penetrates out of the left chamber; the second pipeline is vertically arranged in the right chamber, an injection needle head facing the bottom surface of the coal matrix is arranged at the top end of the second pipeline, and the bottom end of the second pipeline penetrates out of the right chamber; the connecting hose is communicated with the bottom ends of the first pipeline and the second pipeline, and an electric needle valve is installed on the connecting hose.
Preferably, in one of the above-mentioned COs2In the coal-rock component contact angle testing device of the water-coal system, the warm-pressure monitoring system comprises a first pressure sensor installed on the top wall of the left chamber, a second pressure sensor installed on the top wall of the right chamber, and a temperature sensor installed on the right side wall of the right chamber.
Preferably, in one of the above-mentioned COs2In the coal rock component contact angle testing device of the water-coal system, 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 structure principle of the nut valve is the same as that of the ball screw, and the lifting partition plate is driven to lift through the rotation of the nut.
Preferably, in one of the above-mentioned COs2In the coal-rock component contact angle testing device of the water-coal system, the lower part of the right side wall of the right chamber is provided with a discharge pipeline, and a discharge control valve is installed on the discharge pipeline.
Preferably, in one of the above-mentioned COs2In the device for testing the contact angle of the coal-rock component of the water-coal system, 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 CO2A water-coal system coal-rock component contact angle test method using the CO2Testing device for contact angle of coal and rock component of water-coal system for CO under high temperature and high pressure2And (4) detecting the coal-rock component contact of the water-coal system.
According to the technical scheme, compared with the prior art, the invention discloses and provides CO2The invention provides a device and a method for testing contact angles of coal and rock components of a water-coal system, which can directly obtain CO through contact angle measurement2Water-coal system coal-rock component contact angle and capable of directly reacting CO in the system2Gas wetting property.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a testing apparatus according to the present invention;
FIG. 2 is a right side view of a high temperature and high pressure reaction chamber provided by the present invention;
FIG. 3 is a front view of the holder of the present invention;
FIG. 4 is a right side view of the clamp holder provided by the present invention;
figure 5 is a top view of the holder of the present invention.
Wherein:
1-high temperature high pressure reaction chamber; 2-lifting partition plates; 3-a left chamber; 4-a right chamber; 5-a clamping frame; 6-a perspective window; 7-a camera; 8-double shell; 9-oil bath lotion; 10-a circulating oil inlet; 11-a circulating oil return port; 12-oil liquid circulation pipeline; 13-a circulation pump; 14-constant temperature heating device; 15-a graduated scale; 16-a water tank; 17-liquid injection pipe; 18-high pressure injection pump; 19-a liquid injection valve; 20-a stirring motor; 21-a stirring shaft; 22-CO2A gas cylinder; 23-CH4A gas cylinder; 24-a vent line; 25-a booster pump; 26-a pressure reducing valve; 27-constant pressure constant speed pump; 28-electric regulating valve; 29-an air compressor; 30-a bypass control valve; 31-pressure control pipeline; 32-a one-way valve; 33-a first pressure relief valve; 34-a first purge valve; 35-a vacuum pump; 36-vacuum line; 37-vacuum pump control valve; 38-a second pressure relief valve; 39-a second evacuation valve; 40-a first conduit; 41-a second conduit; 42-connecting a hose; 43-an injection needle; 44-electrically operated needle valves; 45-a first pressure sensor; 46-a second pressure sensor; 47-temperature sensor; 48-a nut valve; 49-a discharge conduit; 50-a discharge control valve; 51-a signal receiver; 52-control terminal; 53-coal matrix.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to the attached drawings 1 to 5, the embodiment of the invention discloses a CO2The method for testing the contact angle of the coal and rock component of the water-coal system specifically comprises the following steps:
(1) firstly, selecting coal blocks, cutting coal pieces from large coal blocks, and cutting coal samples into square pieces with the size of about 21mm multiplied by 4 mm.
(2) Grinding and roughly processing the cut coal sample by using 220-320-mesh silicon carbide abrasive paper to remove small scratches; then, 400-10000-mesh silicon carbide sand paper is adopted for fine grinding and wet polishing in sequence.
(3) After the sample is dried at room temperature for not less than 72 hours, the surface roughness is measured with an atomic force microscope or a surface roughness measuring instrument after the surface is cleaned, and the roughness Ra (arithmetic average roughness) value is obtained.
(4) When the Ra value is less than 0.1 μm, the surface polishing of the sample is regarded as qualified and can enter equipment for measurement; if the Ra value is greater than 0.1 μm, further lapping and polishing may be required.
(5) The coal matrix 53 is clamped and fixed to the holder 5 in the right chamber 4. The holder 5 should be positioned in a field of view visible through the see-through window 6. (the see-through windows are arranged 2, one on the right side as in fig. 1 and one on the front side perpendicular to the paper in fig. 1); the holder 5 is shown in a right-hand and front-view configuration in fig. 1. The graduated scale 15 is arranged above the clamping frame 5 in the right and front view, and the positions measured by the contact angles of the coal samples can be positioned in a plane by taking pictures in two directions.
(6) And (3) turning on the constant temperature heating device 14 and the circulating pump 13, turning on the heat lamp and the light source, and stabilizing the temperature 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 ensured to be tightly closed, and the air tightness of the device is ensured to be good.
(8) And opening the vacuum pump 35 and the vacuum pump control valve 37, exhausting the air in the high-temperature and high-pressure reaction chamber 1, and closing the vacuum pump 35 and the vacuum pump control valve 37 after exhausting the air.
(9) The liquid injection valve 19 is opened, the experimental water in the water tank 16 is injected into the left chamber 3 to the first water level line at the upper part in the figure 1 through the liquid injection pipe 17 by the high-pressure injection pump 18, and the injection is stopped when the height is about four fifths of the height of the water tank 16, and the liquid injection valve 19 is closed.
(10) Maintaining the one-way valve 32 in a closed state. The electric control valve 28 was opened, and gas (CO) was injected through the booster pump 25 and the high-precision constant-pressure constant-speed pump 27 (precision 0.01MPa)2Or CH2) (ii) a Gas (CO)2) During the injection process, the electric control stirrer is turned on to stir the liquid in the left chamber 3 to promote CO2And H2The dissolution balance of O; at this time, CO in the left chamber 32Will be partially dissolved in water and the upper part is CO2Gas layer with saturated CO in the lower part2The aqueous layer of (a); the water level in the left chamber 3 is lower than the inlet of the first conduit 40 in the left chamber 3.
(11) In the injection process, a pressure value in the cavity is obtained through a pressure sensor, and when a fixed pressure increment value is set (for example, the pressure interval is set to be 2MPa), the one-way valve 32 is opened at intervals, so that the gas on the upper part of the first water line of the left cavity 3 flows into the right cavity 4 intermittently; the right chamber 4 is gas and the pressure gradually increases.
(12) The pressure in the cavity is gradually increased to a set experimental pressure value (the pressure value is obtained by 2 pressure sensors on the left and right cavities), the booster pump 25 and the electric regulating valve 28 are closed, and the gas injection is stopped.
(13) The electrically controlled stirrer was switched off and left for 5 hours, CO was established in the left chamber 32And H2Dissolution equilibrium and pressure equilibrium 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 pressure, and the right chamber 4 is measured as the whole chamber pressure), and the set pressure value is reached most stably.
(14) If the pressure in the left and right chambers is higher than the set pressure value after being injected carelessly (monitored by 2 high-precision pressure sensors of the left and right chambers), respectively releasing the pressure (selecting a high-precision and electric control valve) to the set pressure (keeping the one-way valve 32 open when releasing, and opening one pressure relief valve) by 2 automatic pressure relief valves communicated with the left and right chambers; if the pressure is too low, the steps 14-15 are repeated.
(15) The nut valve 48 is rotated counterclockwise to lift the lifting clapboard 2 by about 1cm, so that water slowly flows into the right chamber 4 from the lower part of the left chamber 3 along the lifting part at the bottom, and simultaneously, the opening state of the one-way valve 32 is kept, so that the supercritical CO in the right chamber 42Flows into the left chamber 3 (forming an upper gas flow cycle and a lower water flow cycle), and when the levels of the two chambers are at the same height (the liquid level, i.e. the second water level line in the middle of fig. 1, is higher than the coal substrate 53 in the right chamber 4), the device is at rest for about 1 hour; at the moment, the two chambers complete the balance of air pressure and density and saturate CO in water2CO in gas and coal2The gas adsorption is saturated.
(16) The nut valve 48 is rotated clockwise to close the lifting clapboard 2 tightly; 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 pipeline 40 in the left chamber 3; the left and right chambers are not communicated.
(17) Increasing the pressure of the constant pressure constant speed pump 27 by 0.01Mpa based on the set pressure, opening the electric control valve 28, and injecting gas (CO) into the left chamber 3 again2) (ii) a Under the pressure effect of pressurizing 0.01MPa, 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); by opening the electric needle valve 44, CO is in the left chamber 32Gas will enter the right chamber 4 through the conduit via the injection needle 43 (after the left and right chamber conditions are balanced). CO control by controlling the electric needle valve 44 and the injection needle 432The bubbles float upwards in bubble form.
(18) The injection needle 43 is movable up and down, the outer wall of the injection needle is fixed on the wall of the bin, and the inner injection device can realize stepless up and down movement; when CO is present2When sticking to the needle, the injection needle can be pulled down to make CO2The bubbles are separated and float upwards.
(19) When the first measurement is completed, the position of the coal substrate 53 in the holding frame 5 is moved, and the next station test is started.
(20)CO2When the bubbles are extruded out of the needle head, the positions of a right camera and a front camera outside the chamber are adjusted to be opposite to the contact position of the bubbles and the coal, and laser beams are adjusted to irradiate the contact center position of the bubbles; in the whole process, a right camera and a front camera outside the chamber carry out video recording through a transparent high-pressure glass window, and images are extracted for carrying out contact angle measurement calculation.
(21) Calculation of contact angle: and calculating a photograph recorded immediately after the bubbles are contacted with the surface of the coal matrix and are stably balanced, and calculating the static contact angle by using a Young equation. The dynamic contact angle was then further calculated by young's equation using the photograph taken during the movement of the bubble.
(22) Taking out the sample, and drying at normal temperature; photographing through right-hand camera and front-hand camera and positioning CO through holder 5 coordinate system2Contacting the coal-based surface at a specific location. And marking and numbering the measuring points on the surface of the coal matrix.
(23) And (3) placing the sample under a micro photometer, and observing the micro components according to the standard to obtain the micro component information of each measuring point. Further, a scanning electron microscope can be adopted to carry out surface observation on the test position.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
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 (10)
1. CO (carbon monoxide)2-a water-coal system coal-rock component contact angle testing device, characterized by comprising:
a high-temperature high-pressure reaction chamber (1); the outer side of the high-temperature high-pressure reaction cavity (1) is wrapped with a temperature control system; the high-temperature high-pressure reaction cavity (1) is hermetically divided into a left cavity (3) and a right cavity (4) by a lifting clapboard (2); a clamping frame (5) used for clamping a coal matrix (53) is placed 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 erected on the outer side of 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 chamber (3); the aeration system is used for providing CO2And/or CH4A gas;
a pressure control valve circuit; the pressure control valve circuit is positioned outside the high-temperature high-pressure reaction cavity (1), is connected between the left chamber (3) and the right chamber (4), and is used for realizing gas circulation from the left chamber (3) to the right chamber (4);
a bubble pipe line; the air bubble pipeline is communicated with the left chamber (3) and the right chamber (4), one end of the air bubble pipeline is positioned at the upper part of the left chamber (3), the other end of the air bubble pipeline is positioned below the coal matrix (53), and the air bubble pipeline is used for blowing air bubbles to the bottom surface of the coal matrix (53);
a warm pressure monitoring system; the warm-pressing 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).
2. CO according to claim 12-water-coal system coal-rock component contact angle testing device, characterized in that the temperature control system comprises a shapeA double-layer shell (8) formed on the outer side wall of the high-temperature high-pressure reaction cavity (1), wherein an oil bath liquid (9) is filled in a clearance cavity of the double-layer shell (8); the outer side wall of the double-layer shell (8) is provided with a circulating oil inlet (10) and a circulating oil return port (11), the circulating oil inlet (10) and an oil liquid circulating pipeline (12) located on the outer side of the double-layer shell (8) are connected between the circulating oil return port (11), and a circulating pump (13) and a constant-temperature heating device (14) are installed on the oil liquid circulating pipeline (12).
3. CO according to claim 12The water-coal system coal-rock component contact angle testing device is characterized in that the clamping frame (5) is fixed at the middle lower part of the right chamber (4) through a support, 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 chamber (4), the bottom surface of the square tube is axially provided with notches penetrating through two ends, the coal matrix (53) is placed in the square tube, and bubbles expanded from the bubble pipeline are in contact with the bottom surface of the coal matrix (53) through the notches; the top surface of the square pipe faces two of the two edges of the camera (7) are provided with graduated scales (15).
4. CO according to claim 12-a water-coal system coal-rock component contact angle testing device, characterized in that the liquid injection system comprises a water tank (16), the water tank (16) is communicated with the top wall of the left chamber (3) through an 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 chamber (3); the left chamber (3) is also provided with a stirrer; the stirrer comprises a stirring motor (20) and a stirring shaft (21); stirring motor (20) are fixed on the outer roof of left side cavity (3), (mixing) shaft (21) vertical arrangement is in inside left side cavity (3), and the top with the power take off hub connection of stirring motor (20), evenly be fixed with stirring vane on (mixing) shaft (21).
5. CO according to claim 12Coal-rock group of water-coal systemA tap antenna test device, characterized in that the venting system comprises CO2Gas cylinder (22) and CH4A gas cylinder (23); the CO is2Gas cylinder (22) and the CH4The gas cylinders (23) are connected in parallel and then communicated with the bottom wall of the left chamber (3) through a vent pipeline (24); the vent line (24) is connected with the CO2Gas cylinder (22) and the CH4A 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 is2Gas cylinder (22) and the CH4Branch control valves (30) are respectively arranged on the parallel branches of the gas bottle (23).
6. CO according to claim 12-a water-coal system coal-rock component contact angle testing device, characterized in that the pressure control valve circuit comprises a pressure control circuit (31) connected to the top walls of the left chamber (3) and the right chamber (4); a check valve (32) is mounted on the pressure control pipeline (31), and the check valve (32) only enables gas to flow from the left chamber (3) to the right chamber (4); and two parallel branches are arranged on the pressure control pipeline (31) between the one-way valve (32) and the right chamber (4), and a first pressure relief valve (33) and a first emptying valve (34) are respectively arranged on the two branches.
7. CO according to claim 12-a water-coal system coal-rock component contact angle testing device, characterized in that the left chamber (3) is further 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 chamber (3) through a vacuum pipeline (36), and a vacuum pump control valve (37) is installed on the vacuum pipeline (36); and two parallel branches are arranged on the vacuum pipeline (36) between the vacuum pump control valve (37) and the left chamber (3), and a second pressure relief valve (38) and a second exhaust valve (39) are respectively arranged on the two branches.
8. CO according to claim 12Coal-rock component contact angle of water-coal systemThe testing device is characterized in that 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 inside the right chamber (4), the top end of the second pipeline is provided with an injection needle (43) facing the bottom surface of the coal matrix (53), and the bottom end of the second pipeline 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 installed on the connecting hose (42).
9. CO according to claim 12-water-coal system coal-rock component contact angle testing device, characterized in that the warm-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).
10. CO (carbon monoxide)2-method for testing the contact angle of a coal-rock component of a water-coal system, characterized in that a CO according to any one of claims 1 to 9 is used2Testing device for contact angle of coal and rock component of water-coal system for CO under high temperature and high pressure2And (4) detecting the coal-rock component contact of the water-coal system.
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