CN111175218B - Supercritical carbon dioxide extraction-permeability testing device and method - Google Patents
Supercritical carbon dioxide extraction-permeability testing device and method Download PDFInfo
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- CN111175218B CN111175218B CN202010208921.2A CN202010208921A CN111175218B CN 111175218 B CN111175218 B CN 111175218B CN 202010208921 A CN202010208921 A CN 202010208921A CN 111175218 B CN111175218 B CN 111175218B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/0866—Sorption
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- 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 relates to a supercritical carbon dioxide extraction-permeability testing device, which comprises a carbon dioxide gas source, a purifier, a condenser, a carrying metering barrel, a carbon dioxide flowmeter, a carrying agent pump, a high-pressure carbon dioxide pump, a mixer, an extraction kettle and a clamp, wherein the carbon dioxide gas source is communicated with the purifier through a guide pipe, the purifier is respectively communicated with the condenser and a separation kettle II through a guide pipe, and the condenser is respectively communicated with the high-pressure carbon dioxide pump and the carrying agent pump through guide pipes. The test method comprises the steps of equipment assembly, equipment prefabrication, air tightness detection, experiment prefabrication, extraction experiments, seepage experiments and the like. The supercritical extraction CO2 and permeability test under the in-situ reservoir condition can be carried out, coal adsorption, extraction and permeability experiments of different states such as columnar coal, coal powder and the like can be carried out, the extraction solution can be sampled, concentrated and distilled without transferring a sample, the loss of effective substances is reduced, and the extraction efficiency and the accuracy are improved.
Description
Technical Field
The invention relates to a supercritical carbon dioxide extraction-permeability testing device, belonging to the technical field of coal bed gas experimental research equipment.
Background
The research of supercritical carbon dioxide extraction mainly focuses on the improvement of supercritical carbon dioxide on coal. The supercritical carbon dioxide is a good supercritical solvent, can extract organic micromolecules in the coal to change the physical and chemical properties of the coal, and changes the gas adsorption capacity and essence of the coal. In the coal chemistry research, a solvent is used for extracting, and the small molecular phase in the coal is released by utilizing the electron donating and accepting capability of the solvent, so that the separation of a main body and an object of a coal structure is achieved, and a structural model of the coal and the influence of the structural model on the properties of the coal are presumed and verified. The micromolecule phase is separated from the macromolecular network structure step by step through extraction, and the analysis of soluble matters and insoluble matters in different solvents can provide a large amount of basis for the establishment and verification of a coal structure model on one hand, and the quantity of micromolecules in the extract also represents the stability of the physical and chemical properties of coal to a certain extent on the other hand.
Gas in a coal seam mainly exists in an adsorption state, but the complexity of pore cracking of a coal reservoir is high, the coal reservoir also has low permeability, and reservoir strengthening measures such as hydraulic fracturing and acid fracturing are often adopted in the current coal seam gas ground development practice to increase the permeability of the reservoir. Although researchers at home and abroad do a lot of experiments and researches on the solvent extraction of coal, mainly used for the research on coal chemistry and coal structure, a simulation experiment device and a research method which can be directly used for improving reservoir conditions by combining the supercritical carbon dioxide extraction with the permeability test of coal are not available. In view of the fact that the conventional hydraulic fracturing and gas flooding method is only relied on in the current coal bed gas development process, the obtained effect is not obvious, and a new reservoir strengthening process measure needs to be searched urgently to improve the physical property of the reservoir, so that the productivity of the coal bed gas well is increased.
Disclosure of Invention
The invention aims to overcome the defects and provide a supercritical carbon dioxide extraction-permeability testing device and method.
In order to realize the purpose, the invention is realized by the following technical scheme:
a supercritical carbon dioxide extraction-permeability testing device comprises a carbon dioxide gas source, a purifier, a condenser, a carrying metering tank, a carbon dioxide flowmeter, a carrying agent pump, a high-pressure carbon dioxide pump, a mixer, an extraction kettle, a clamp, a preheater I, a preheater II, a preheater III, a separation kettle I, a separation kettle II, a carrying agent flowmeter, a thermometer, a pressure gauge and a safety valve, wherein the carbon dioxide gas source is communicated with the purifier through a guide pipe, the purifier is respectively communicated with the condenser and the separation kettle II through the guide pipe, the condenser is respectively communicated with the high-pressure carbon dioxide pump and the carrying agent pump through the guide pipe, the high-pressure carbon dioxide pump and the carrying agent pump are respectively communicated with the guide pipe through a one-way valve, the high-pressure carbon dioxide pump and the carrying agent pump are mutually connected in series, and the carrying agent pump is communicated with the carrying metering tank through the guide pipe, and a flow guide pipe between the carrying metering barrel and the carrying agent pump is provided with a carrying agent flow meter, the mixer is communicated with the high-pressure carbon dioxide pump and the flow guide pipe between the check valves connected with the carrying agent pump through the flow guide pipe, the mixer is communicated with a preheater I through a guide pipe, the preheater I is respectively connected with the extraction kettle and the holder through the guide pipe, the holder is further communicated with the extraction kettle and the preheater II through a guide pipe, the extraction kettle is further communicated with the preheater II through a guide pipe, the preheater II is communicated with the separation kettle I through a guide pipe, the separation kettle I is communicated with the preheater III through a guide pipe, the preheater III is communicated with the separation kettle II through a guide pipe, and the guide pipes between the extraction kettle and the preheater II and between the separation kettle I and the preheater III are respectively connected with a thermometer, a manometer and a safety valve.
Further, the holder includes vacuum pump, buffer tank, auxiliary pump, detection chamber, wherein detect chamber anterior segment face and pass through honeycomb duct and I intercommunication of preheater, and the rear end face passes through honeycomb duct and II intercommunications of extraction cauldron and preheater, the vacuum pump passes through buffer tank and the preceding terminal surface intercommunication in detection chamber and communicates with I intercommunication of preheater, the auxiliary pump totally two to communicate with the detection chamber respectively, and two auxiliary pumps and detection chamber intercommunication position are in order to detect the middle point symmetric distribution in the chamber, all establish a pressure gauge between the honeycomb duct that detects chamber and buffer tank, auxiliary pump intercommunication.
Furthermore, the detection cavity comprises a detection barrel body, a front end cover, a rear end cover, an auxiliary baffle ring, a guide sleeve, a driving piston, a front core chamber, a rear core chamber, a bearing rubber sleeve, an elastic cushion plate, a strain gauge and a displacement sensor, the charging barrel is of a cylindrical hollow tubular structure, the rear end face of the charging barrel is connected with the rear end cover, the front end face of the charging barrel is connected with the guide sleeve and is connected with the front end cover through the guide sleeve, the detection barrel body, the front end cover, the rear end cover and the guide sleeve are coaxially distributed, the front core chamber and the rear core chamber are of a convex columnar structure, the diameter of the front end face of the charging barrel is at least 3 times that of the rear end face, the front end faces of the front core chamber and the rear core chamber are embedded in the detection barrel body, the rear end face is positioned outside the front end cover and the rear core chamber and the detection barrel body are coaxially distributed, a flow guide cavity coaxially distributed with the detection barrel body is arranged in the front core chamber and the rear core chamber, the flow guide cavity is respectively communicated with the preheater I, the extraction kettle and the preheater II through flow guide pipes, the front core chamber is in sliding connection with the front end cover and the detection barrel through auxiliary baffle rings and is abutted against a driving piston, the driving piston is embedded in the front end cover and is positioned between the front end cover and the guide sleeve and coaxially distributed with the detection barrel, the front core chamber is coated outside the front core chamber and is in sliding connection with the guide sleeve, at least one axial pressurizing opening is formed in the side surface of the front end cover corresponding to the rear end surface of the driving piston, an axial pressure relief opening is formed in the outer side surface of the guide sleeve corresponding to the front end surface of the driving piston, the axial pressurizing opening and the axial pressure relief opening are respectively communicated with the driving piston and are communicated with an auxiliary pump through the flow guide pipes, the bearing rubber sleeve is embedded in the detection barrel and coaxially distributed with the detection barrel and is abutted against the inner side surface of the detection barrel, and two ends of the bearing rubber sleeve are respectively connected with the auxiliary baffle rings at two ends of the detection barrel and coated on the front core chamber, The front end surfaces of the front core chamber and the rear core chamber are correspondingly provided with bearing chambers with the length of 1/3-2/3 of the detection cylinder body in the length direction, the elastic backing plate and the strain gauge are both positioned in the bearing chambers, the elastic backing plate is propped against the front end face of the back core chamber and is coaxially distributed, the side wall of the bearing chamber corresponding to the detection cylinder body is provided with a detection port and an annular pressurizing port, wherein the detection port is connected with the thermometer, the annular pressurizing port is communicated with the gap between the bearing rubber sleeve and the detection cylinder body, at the same time, the device is communicated with an auxiliary pump through a flow guide pipe, at least one strain gauge is arranged, each strain gauge is provided with a lead and is electrically connected with the lead, and the other end of the lead is positioned outside the detection cylinder body through the rear end cover, and the displacement sensor is positioned outside the detection cylinder body and is connected with the outer side surface of the outer side part of the detection cylinder body, which is positioned in the front core chamber.
Further, accuse honeycomb duct and carbon dioxide air supply, clarifier, condenser, carry measuring bucket, carbon dioxide flowmeter, carry agent pump, high-pressure carbon dioxide pump, blender, extraction cauldron, holder, preheater I, preheater II, preheater III, separation cauldron I, separation cauldron are connected through the control valve between II, just all establish at least one thermometer and pressure gauge on clarifier, condenser, blender, extraction cauldron, holder, preheater I, preheater II, preheater III, separation cauldron I, the separation cauldron II.
Further, the holder department establishes control circuit, control circuit respectively with carbon dioxide air supply, clarifier, condenser, carry measuring tank, carbon dioxide flowmeter, carry agent pump, high-pressure carbon dioxide pump, blender, extraction cauldron, holder, preheater I, preheater II, preheater III, separation cauldron I, separation cauldron II and control valve electrical connection.
Furthermore, the control circuit is a circuit system based on any one of a programmable controller, an industrial single chip microcomputer and an internet-of-things controller.
A test method of a supercritical carbon dioxide extraction-permeability test device comprises the following steps:
s1, assembling equipment, namely, electrically connecting a carbon dioxide gas source, a purifier, a condenser, a carrying metering barrel, a carbon dioxide flowmeter, a carrying agent pump, a high-pressure carbon dioxide pump, a mixer, an extraction kettle, a clamp, a preheater I, a preheater II, a preheater III, a separation kettle I, a separation kettle II and a control valve for later use according to use requirements;
s2, prefabricating equipment, after the step S1 is completed, firstly crushing the collected coal sample according to the requirement of detection operation, then compacting the crushed coal scraps to prepare a cylindrical coal sample with the length of 50mm and the diameter of 50mm, then setting the experiment temperature and the experiment pressure of the detection operation according to the metal type sample block with the same diameter and length and the detection requirement;
s3, performing air tightness detection, namely after the detection operation in the step S2 is completed, firstly installing the metal type sample block prepared in the step S2 into a bearing chamber of a clamp holder, connecting the metal type sample block with the front end face of the rock core chamber behind the clamp holder and coaxially distributing the metal type sample block, then driving an auxiliary pump to operate, adjusting a driving piston to operate, driving the front rock core chamber to operate by the driving piston and clamping and positioning the other end of the metal type sample block, then evacuating the air in the clamp holder through a vacuum pump, enabling the pressure value in the clamp holder to reach-0.19 MPa, and maintaining the pressure for 2-4 hours to complete the air tightness detection;
s4, performing experiment prefabrication, taking out the metal type sample block from the clamp holder after the detection operation of the step S3 is completed, installing the coal sample prepared in the step S2 into the hardness holder, evacuating the air in the clamp holder through the vacuum pump again, enabling the pressure value in the clamp holder to reach-0.19 MPa, and maintaining the pressure; then respectively driving a carbon dioxide gas source, a condenser, a high-pressure carbon dioxide pump, a mixer, an extraction kettle, a preheater II, a preheater III, a separation kettle I and a separation kettle II to operate, on one hand, adjusting the operation temperature of the condenser, the mixer, the extraction kettle, the preheater II, the preheater III, the separation kettle I and the separation kettle II to reach the set experimental value in the step S2, on the other hand, driving the high-pressure carbon dioxide pump to operate, pressurizing the carbon dioxide device conveyed by the carbon dioxide gas source, conveying the carbon dioxide into a clamp holder after the temperature and pressure of the condenser and the mixer are adjusted, enabling the air pressure and the temperature in the clamp holder to reach the set experimental value in the step S2, and carrying out subsequent operation after the air pressure and the temperature in the clamp holder reach the set experimental value in the step S2 and carrying out heat preservation and pressure maintenance for 1-3 minutes;
s5, performing an extraction experiment, after the step S4 is completed, communicating a clamp holder with external carbon dioxide gas, disconnecting the clamp holder from an extraction kettle and a preheater II and maintaining pressure, increasing the air pressure in the clamp holder to a set value in the step S2 through an auxiliary pump of a carrying agent pump, a high-pressure carbon dioxide pump and the clamp holder, maintaining the pressure for 96 hours, finally disconnecting the clamp holder from the carbon dioxide gas, taking out a coal sample, naturally cooling the coal sample and the clamp holder to room temperature, weighing and measuring the coal sample on one hand, returning to the step S4 on the other hand, installing a brand new coal sample in the clamp holder, and performing a subsequent experiment;
s6, after the seepage experiment is completed and the step S5 is completed, reading the numerical values of a carbon dioxide flowmeter, a thermometer on a flow guide pipe, a manometer and a thermometer and a manometer at a holder and starting to continuously record; then driving the carrier pump, the high-pressure carbon dioxide pump and the auxiliary pump of the holder to operate, increasing the temperature and the pressure in the holder, firstly increasing the air pressure in the holder to 0.1-0.4 MPa, increasing the temperature to 25-45 ℃, then continuously supplying carbon dioxide gas into the holder, keeping the temperature and the air pressure in the holder to stably operate for 12 hours to achieve adsorption balance, and continuously recording the pressure and the temperature value in the adsorption process; and after the adsorption balance is finished, the pressure value of the carbon dioxide conveyed into the holder is increased to reach 0.4-0.8, the holder is communicated with the extraction kettle and the preheater II, and after the pressure value is kept to stably operate for 5 minutes, data continuous acquisition is started through the pressure and the thermometer, so that the extraction experiment can be finished.
Further, in the step S2, the experimental preset temperature of the condenser is 5 ℃, the conveying pressure of the high-pressure carbon dioxide pump is 10MPa, and the rotating speed is 30 r/min; the critical temperature of the carbon dioxide in the holder is 31.1 ℃, the critical pressure is 7.38 MPa, the experimental temperature is 32 ℃, the extraction pressure is 10MPa, and the experimental time of extraction is set to be 96 hours.
The invention has simple structure, convenient operation, multiple purposes and good universality, can carry out supercritical extraction CO2 and permeability test under the condition of an in-situ reservoir, can also carry out coal body adsorption, extraction and permeability experiments of different states such as columnar, briquette coal, pulverized coal and the like, can combine the universality and the high efficiency of high-temperature and high-pressure extraction and the high selectivity of solid phase extraction, realizes the material extraction under the high-temperature and high-pressure state and in a closed space, can test the permeability of a sample by pressurization/decompression control and regulation, and can also carry out sampling, concentration and distillation on an extraction solution without transferring the sample, thereby reducing the loss of effective materials and improving the extraction efficiency and the accuracy.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of a partial structure of a detection chamber;
FIG. 3 is a flow chart of the test method of the present invention.
Detailed Description
The invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the description of the embodiments is only for illustrating the present invention and should not be taken as limiting the invention as detailed in the claims.
As shown in figures 1 and 2, a supercritical carbon dioxide extraction-permeability testing device comprises a carbon dioxide gas source 1, a purifier 2, a condenser 3, a carrying metering tank 4, a carbon dioxide flow meter 5, a carrying agent pump 6, a high-pressure carbon dioxide pump 7, a mixer 8, an extraction kettle 10, a clamp 9, a preheater I11, a preheater II 12, a preheater III 13, a separation kettle I14, a separation kettle II 15, a carrying agent flow meter 16, a thermometer 17, a pressure gauge 18 and a safety valve 19, wherein the carbon dioxide gas source 1 is communicated with the purifier 2 through a flow guide pipe, the purifier 2 is respectively communicated with the condenser 3 and the separation kettle II 15 through the flow guide pipe, the condenser 2 is respectively communicated with the high-pressure carbon dioxide pump 7 and the carrying agent pump 6 through the flow guide pipe, the high-pressure carbon dioxide pump 7 and the carrying agent pump 6 are respectively communicated with the flow guide pipe through a one-way valve 20, and the high-pressure carbon dioxide pump 7, The carrying agent pump 6 is connected in series, the carrying agent pump 6 is communicated with the carrying metering barrel 4 through a guide pipe, a carrying agent flowmeter 16 is arranged on the guide pipe between the carrying metering barrel 4 and the carrying agent pump 6, the mixer 8 is communicated with the guide pipe between the high-pressure carbon dioxide pump 7 and the one-way valve 20 connected with the carrying agent pump 6 through the guide pipe, the mixer 8 is communicated with the preheater I11 through the guide pipe, the preheater I11 is respectively connected with the extraction kettle 10 and the clamper 9 through the guide pipe, the clamper 9 is communicated with the extraction kettle 10 and the preheater II 12 through the guide pipe, the extraction kettle 10 is communicated with the preheater II 12 through the guide pipe, the preheater II 12 is communicated with the separation kettle I14 through the guide pipe, the separation kettle I14 is communicated with the preheater III 13 through the guide pipe, the preheater III 13 is communicated with the separation kettle II 15 through the guide pipe, the flow guide pipes between the extraction kettle 10 and the preheater II 12 and between the separation kettle I14 and the preheater III 13 are respectively connected with a thermometer 17, a pressure gauge 18 and a safety valve 19.
It is emphasized that the holder 9 includes a vacuum pump 91, a buffer tank 92, an auxiliary pump 93, and a detection chamber 94, wherein the front end surface of the detection chamber 94 is communicated with the preheater i 11 through a flow guide tube, the rear end surface is communicated with the extraction kettle 10 and the preheater ii 12 through a flow guide tube, the vacuum pump 91 is communicated with the front end surface of the detection chamber 94 through the buffer tank 92 and is communicated with the preheater i 11, the auxiliary pumps 93 are two in number and are respectively communicated with the detection chamber 94, the communication positions of the two auxiliary pumps 93 and the detection chamber 94 are symmetrically distributed at the midpoint of the detection chamber 94, and a pressure gauge 18 is disposed between the flow guide tubes communicating the detection chamber 94 with the buffer tank 92 and the auxiliary pumps 93.
It is worth noting that the detection cavity 94 comprises a detection cylinder 941, a front end cover 942, a rear end cover 943, an auxiliary baffle ring 944, a guide sleeve 945, a driving piston 946, a front core chamber 947, a rear core chamber 948, a rubber bearing sleeve 949, an elastic cushion 940, a strain gauge 9401 and a displacement sensor 9402, wherein the detection cylinder 941 is of a cylindrical hollow tubular structure, the rear end face of the detection cylinder 941 is connected with the rear end cover 943, the front end face of the detection cylinder 941 is connected with the guide sleeve 945 and is connected with the front end cover 942 through the guide sleeve 945, the detection cylinder 941, the front end cover 942, the rear end cover 943 and the guide sleeve 945 are coaxially distributed, the front core chamber 947 and the rear core chamber 948 are of a convex cylindrical structure, the diameter of the front end face of the detection cylinder is at least 3 times of the diameter of the rear end face, the front core chamber 947 and the rear core chamber 948 are both embedded in the detection cylinder 941, the rear end face of the detection cylinder 942 is located outside the front end cover 942 and the rear core chamber 943 are coaxially distributed with the detection cylinder 941, a guide cavity 9403 which is coaxially distributed with the detection cylinder 941 is arranged in the front rock ventricle 947 and the rear rock ventricle 948, the guide cavity 9403 is respectively communicated with the pre-heater I11, the extraction kettle 10 and the pre-heater II 12 through guide pipes, the front rock ventricle 947 is in sliding connection with the front end cover 942 and the detection cylinder 941 through an auxiliary retaining ring 944 and abuts against a driving piston 946, the driving piston is embedded in the front end cover 946, is positioned between the front end cover 942 and the guide sleeve 945 and is coaxially distributed with the detection cylinder 941, is coated outside the front rock ventricle 947 and is in sliding connection with the guide sleeve 945, at least one axial pressurization hole 9404 is arranged on the side surface of the front end cover 942 corresponding to the rear end surface of the driving piston 946, an axial pressure relief hole 9405 is arranged on the outer side surface of the guide sleeve 945 corresponding to the front end surface of the driving piston 946, the axial pressurization 9404 and the axial pressure relief hole 9405 are respectively communicated with the driving piston 946 and are communicated with an auxiliary pump 93 through a guide pipe, bear gum cover 949 inlay in detecting barrel 941 with detect barrel 941 coaxial distribution and with detect barrel 941 medial surface and offset, and bear the weight of gum cover 949 both ends respectively with detect the supplementary fender ring 944 connection and the cladding of barrel 941 both ends position in the front of rock ventricle 947, back rock ventricle 948 lateral surface, preceding rock ventricle 947, back rock ventricle 948 front end face are established length for detecting barrel 941 length 1/3-2/3 load-bearing chamber 9405 in corresponding detection barrel 941, elastic backing plate 940 and foil gage 9401 all are located load-bearing chamber 9405, and elastic backing plate 940 offsets and coaxial distribution with back rock ventricle 948 front end face, load-bearing chamber 9405 corresponds and is established one on the detection barrel 941 lateral wall and detects a detection mouth 9406 and an annular pressure boost mouth 9407, wherein detect mouth 9406 and be connected with thermometer 17, annular pressure boost mouth 9407 communicates with bearing gum cover 949 and the clearance between the detection barrel 941, passes through the honeycomb duct intercommunication with an auxiliary pump 93 simultaneously, the foil gage 9401 is at least one, and each foil gage 9401 all establishes a wire 9408 and with wire 9408 electrical connection, and the wire other end is located the detection barrel 941 outside through rear end cover 943, displacement sensor 9402 is located the detection barrel 941 outside to be located the detection barrel 941 outside lateral surface with preceding rock ventricle 947 and be connected.
In addition, the control honeycomb duct is connected with a carbon dioxide gas source 1, a purifier 2, a condenser 3, a carrying metering barrel 4, a carbon dioxide flowmeter 5, a carrying agent pump 6, a high-pressure carbon dioxide pump 7, a mixer 8, an extraction kettle 10, a holder 9, a preheater I11, a preheater II 12, a preheater III 13, a separation kettle I14 and a separation kettle II 15 through a control valve 21, and at least one thermometer 17 and a pressure gauge 18 are arranged on the purifier 2, the condenser 3, the mixer 8, the extraction kettle 10, the holder 9, the preheater I11, the preheater II 12, the preheater III 13, the separation kettle I14 and the separation kettle II 15.
Meanwhile, the holder 9 is provided with a control circuit 22, and the control circuit 22 is respectively electrically connected with a carbon dioxide gas source 1, a purifier 2, a condenser 3, a carrying metering barrel 4, a carbon dioxide flowmeter 5, a carrying agent pump 6, a high-pressure carbon dioxide pump 7, a mixer 8, an extraction kettle 10, a holder 9, a preheater I11, a preheater II 12, a preheater III 13, a separation kettle I14, a separation kettle II and a control valve 21.
Preferably, the control circuit 22 is a circuit system based on any one of a programmable controller, an industrial single chip, and an internet-of-things controller.
As shown in fig. 3, a testing method of a supercritical carbon dioxide extraction-permeability testing apparatus includes the following steps:
s1, assembling equipment, namely electrically connecting a carbon dioxide gas source, a purifier, a condenser, a carrying metering barrel, a carbon dioxide flowmeter, a carrying agent pump, a high-pressure carbon dioxide pump, a mixer, an extraction kettle, a clamp, a preheater I, a preheater II, a preheater III, a separation kettle I, a separation kettle II and a control valve for later use according to use requirements;
s2, prefabricating equipment, after the step S1 is completed, firstly crushing the collected coal sample according to the requirement of detection operation, then compacting the crushed coal scraps to prepare a cylindrical coal sample with the length of 50mm and the diameter of 50mm, then setting the experiment temperature and the experiment pressure of the detection operation according to the metal type sample block with the same diameter and length and the detection requirement;
s3, performing air tightness detection, namely after the detection operation in the step S2 is completed, firstly installing the metal type sample block prepared in the step S2 into a bearing chamber of a clamp holder, connecting the metal type sample block with the front end face of the rock core chamber behind the clamp holder and coaxially distributing the metal type sample block, then driving an auxiliary pump to operate, adjusting a driving piston to operate, driving the front rock core chamber to operate by the driving piston and clamping and positioning the other end of the metal type sample block, then evacuating the air in the clamp holder through a vacuum pump, enabling the pressure value in the clamp holder to reach-0.19 MPa, and maintaining the pressure for 2-4 hours to complete the air tightness detection;
s4, performing experiment prefabrication, taking out the metal type sample block from the clamp holder after the detection operation of the step S3 is completed, installing the coal sample prepared in the step S2 into the hardness holder, evacuating the air in the clamp holder through the vacuum pump again, enabling the pressure value in the clamp holder to reach-0.19 MPa, and maintaining the pressure; then respectively driving a carbon dioxide gas source, a condenser, a high-pressure carbon dioxide pump, a mixer, an extraction kettle, a preheater II, a preheater III, a separation kettle I and a separation kettle II to operate, on one hand, adjusting the operation temperature of the condenser, the mixer, the extraction kettle, the preheater II, the preheater III, the separation kettle I and the separation kettle II to reach the set experimental value in the step S2, on the other hand, driving the high-pressure carbon dioxide pump to operate, pressurizing the carbon dioxide device conveyed by the carbon dioxide gas source, conveying the carbon dioxide into a clamp holder after the temperature and pressure of the condenser and the mixer are adjusted, enabling the air pressure and the temperature in the clamp holder to reach the set experimental value in the step S2, and carrying out subsequent operation after the air pressure and the temperature in the clamp holder reach the set experimental value in the step S2 and carrying out heat preservation and pressure maintenance for 1-3 minutes;
s5, performing an extraction experiment, after the step S4 is completed, communicating a clamp holder with external carbon dioxide gas, disconnecting the clamp holder from an extraction kettle and a preheater II and maintaining pressure, increasing the air pressure in the clamp holder to a set value in the step S2 through an auxiliary pump of a carrying agent pump, a high-pressure carbon dioxide pump and the clamp holder, maintaining the pressure for 96 hours, finally disconnecting the clamp holder from the carbon dioxide gas, taking out a coal sample, naturally cooling the coal sample and the clamp holder to room temperature, weighing and measuring the coal sample on one hand, returning to the step S4 on the other hand, installing a brand new coal sample in the clamp holder, and performing a subsequent experiment;
s6, after the seepage experiment is completed and the step S5 is completed, reading the numerical values of a carbon dioxide flowmeter, a thermometer on a flow guide pipe, a manometer and a thermometer and a manometer at a holder and starting to continuously record; then driving the carrier pump, the high-pressure carbon dioxide pump and the auxiliary pump of the holder to operate, increasing the temperature and the pressure in the holder, firstly increasing the air pressure in the holder to 0.1-0.4 MPa, increasing the temperature to 25-45 ℃, then continuously supplying carbon dioxide gas into the holder, keeping the temperature and the air pressure in the holder to stably operate for 12 hours to achieve adsorption balance, and continuously recording the pressure and the temperature value in the adsorption process; and after the adsorption balance is finished, the pressure value of the carbon dioxide conveyed into the holder is increased to reach 0.4-0.8, the holder is communicated with the extraction kettle and the preheater II, and after the pressure value is kept to stably operate for 5 minutes, data continuous acquisition is started through the pressure and the thermometer, so that the extraction experiment can be finished.
Further optimally, in the step S2, the experimental preset temperature of the condenser is 5 ℃, the conveying pressure of the high-pressure carbon dioxide pump is 10MPa, and the rotating speed is 30 r/min; the critical temperature of the carbon dioxide in the holder is 31.1 ℃, the critical pressure is 7.38 MPa, the experimental temperature is 32 ℃, the extraction pressure is 10MPa, and the experimental time of extraction is set to be 96 hours.
The invention has simple structure, convenient operation, multiple purposes and good universality, can carry out supercritical extraction CO2 and permeability test under the condition of an in-situ reservoir, can also carry out coal body adsorption, extraction and permeability experiments of different states such as columnar, briquette coal, pulverized coal and the like, can combine the universality and the high efficiency of high-temperature and high-pressure extraction and the high selectivity of solid phase extraction, realizes the material extraction under the high-temperature and high-pressure state and in a closed space, can test the permeability of a sample by pressurization/decompression control and regulation, and can also carry out sampling, concentration and distillation on an extraction solution without transferring the sample, thereby reducing the loss of effective materials and improving the extraction efficiency and the accuracy.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A supercritical carbon dioxide extraction-permeability testing device is characterized in that: the supercritical carbon dioxide extraction-permeability testing device comprises a carbon dioxide gas source, a purifier, a condenser, a carrying metering barrel, a carbon dioxide flowmeter, a carrying agent pump, a high-pressure carbon dioxide pump, a mixer, an extraction kettle, a clamp, a preheater I, a preheater II, a preheater III, a separation kettle I, a separation kettle II, a carrying agent flowmeter, a thermometer, a pressure gauge and a safety valve, wherein the carbon dioxide gas source is communicated with the purifier through a guide pipe, the purifier is respectively communicated with the condenser and the separation kettle II through the guide pipe, the condenser is respectively communicated with the high-pressure carbon dioxide pump and the carrying agent pump through the guide pipe, the high-pressure carbon dioxide pump and the carrying agent pump are respectively communicated with the guide pipe through a one-way valve, the high-pressure carbon dioxide pump and the carrying agent pump are mutually connected in series, and the carrying agent pump is communicated with the carrying metering barrel through the guide pipe, and a flow guide pipe between the carrying metering barrel and the carrying agent pump is provided with a carrying agent flow meter, the mixer is communicated with the high-pressure carbon dioxide pump and the flow guide pipe between the check valves connected with the carrying agent pump through the flow guide pipe, the mixer is communicated with a preheater I through a guide pipe, the preheater I is respectively connected with the extraction kettle and the holder through the guide pipe, the holder is further communicated with the extraction kettle and the preheater II through a guide pipe, the extraction kettle is further communicated with the preheater II through a guide pipe, the preheater II is communicated with the separation kettle I through a guide pipe, the separation kettle I is communicated with the preheater III through a guide pipe, the preheater III is communicated with the separation kettle II through a guide pipe, and the guide pipes between the extraction kettle and the preheater II and between the separation kettle I and the preheater III are respectively connected with a thermometer, a manometer and a safety valve.
2. The apparatus for supercritical carbon dioxide extraction-permeability testing as claimed in claim 1, wherein: the holder includes vacuum pump, buffer tank, auxiliary pump, detection chamber, wherein detect chamber anterior segment face and pass through honeycomb duct and I intercommunication of preheater, and the rear end face passes through honeycomb duct and extraction cauldron and II intercommunications of preheater, the vacuum pump passes through buffer tank and detects the preceding terminal surface intercommunication in chamber and with I intercommunication of preheater, the auxiliary pump is totally two to communicate with the detection chamber respectively, and two auxiliary pumps and detection chamber intercommunication position are in order to detect the chamber mid point symmetric distribution, all establish a pressure gauge between the honeycomb duct that detects chamber and buffer tank, auxiliary pump intercommunication.
3. The apparatus for supercritical carbon dioxide extraction-permeability testing as claimed in claim 2, wherein: the detection cavity comprises a detection barrel body, a front end cover, a rear end cover, an auxiliary baffle ring, a guide sleeve, a driving piston, a front core chamber, a rear core chamber, a bearing rubber sleeve, an elastic cushion plate, a strain gauge and a displacement sensor, wherein the detection barrel body is of a cylindrical hollow tubular structure, the rear end face of the detection barrel body is connected with the rear end cover, the front end face of the detection barrel body is connected with the guide sleeve and is connected with the front end cover through the guide sleeve, the detection barrel body, the front end cover, the rear end cover and the guide sleeve are coaxially distributed, the front core chamber and the rear core chamber are of a convex columnar structure, the diameter of the front end face of the detection barrel body is at least 3 times that of the rear end face, the front end faces of the front core chamber and the rear core chamber are embedded in the detection barrel body, the rear end face is positioned outside the front end cover and the front core chamber and the rear core chamber are coaxially distributed with the detection barrel body, a flow guide cavity coaxially distributed with the detection barrel body is arranged in the front core chamber and the rear core chamber, the flow guide cavity is respectively communicated with the preheater I, the extraction kettle and the preheater II through flow guide pipes, the front core chamber is in sliding connection with the front end cover and the detection barrel through auxiliary baffle rings and is abutted against a driving piston, the driving piston is embedded in the front end cover and is positioned between the front end cover and the guide sleeve and coaxially distributed with the detection barrel, the front core chamber is coated outside the front core chamber and is in sliding connection with the guide sleeve, at least one axial pressurizing opening is formed in the side surface of the front end cover corresponding to the rear end surface of the driving piston, an axial pressure relief opening is formed in the outer side surface of the guide sleeve corresponding to the front end surface of the driving piston, the axial pressurizing opening and the axial pressure relief opening are respectively communicated with the driving piston and are communicated with an auxiliary pump through the flow guide pipes, the bearing rubber sleeve is embedded in the detection barrel and coaxially distributed with the detection barrel and is abutted against the inner side surface of the detection barrel, and two ends of the bearing rubber sleeve are respectively connected with the auxiliary baffle rings at two ends of the detection barrel and coated on the front core chamber, The front end surfaces of the front core chamber and the rear core chamber are correspondingly provided with bearing chambers with the length of 1/3-2/3 of the detection cylinder body in the length direction, the elastic backing plate and the strain gauge are both positioned in the bearing chambers, the elastic backing plate is abutted against the front end face of the rear core chamber and is coaxially distributed, the side wall of the bearing chamber corresponding to the detection cylinder body is provided with a detection port and an annular pressurizing port, wherein the detection port is connected with the thermometer, the annular pressurizing port is communicated with the gap between the bearing rubber sleeve and the detection cylinder body, at the same time, the device is communicated with an auxiliary pump through a flow guide pipe, at least one strain gauge is arranged, each strain gauge is provided with a lead and is electrically connected with the lead, and the other end of the lead is positioned outside the detection cylinder body through the rear end cover, and the displacement sensor is positioned outside the detection cylinder body and is connected with the outer side surface of the outer side part of the detection cylinder body, which is positioned in the front core chamber.
4. The apparatus for supercritical carbon dioxide extraction-permeability testing as claimed in claim 1, wherein: the honeycomb duct is connected through the control valve with carbon dioxide air supply, clarifier, condenser, carry measuring vessel, carbon dioxide flowmeter, carry agent pump, high-pressure carbon dioxide pump, blender, extraction cauldron, holder, preheater I, preheater II, preheater III, separation cauldron I, separation cauldron II within a definite time, just all establish at least one thermometer and pressure gauge on clarifier, condenser, blender, extraction cauldron, holder, preheater I, preheater II, preheater III, separation cauldron I, the separation cauldron II.
5. The apparatus for supercritical carbon dioxide extraction-permeability testing as claimed in claim 1, wherein: the clamp holder is provided with a control circuit, and the control circuit is respectively electrically connected with a carbon dioxide gas source, a purifier, a condenser, a carrying metering tank, a carbon dioxide flowmeter, a carrying agent pump, a high-pressure carbon dioxide pump, a mixer, an extraction kettle, the clamp holder, a preheater I, a preheater II, a preheater III, a separation kettle I, a separation kettle II and a control valve.
6. The apparatus for supercritical carbon dioxide extraction-permeability testing as claimed in claim 5, wherein: the control circuit is a circuit system based on any one of a programmable controller, an industrial single chip microcomputer and an internet-of-things controller.
7. A test method of a supercritical carbon dioxide extraction-permeability test device is characterized by comprising the following steps:
s1, assembling equipment, namely, electrically connecting a carbon dioxide gas source, a purifier, a condenser, a carrying metering barrel, a carbon dioxide flowmeter, a carrying agent pump, a high-pressure carbon dioxide pump, a mixer, an extraction kettle, a clamp, a preheater I, a preheater II, a preheater III, a separation kettle I, a separation kettle II and a control valve for later use according to use requirements;
s2, prefabricating equipment, after the step S1 is completed, firstly crushing the collected coal sample according to the requirement of detection operation, then compacting the crushed coal scraps to prepare a cylindrical coal sample with the length of 50mm and the diameter of 50mm, then setting the experiment temperature and the experiment pressure of the detection operation according to the metal type sample block with the same diameter and length and the detection requirement;
s3, detecting air tightness, after the detection operation of the S2 step is completed, firstly installing the metal type sample block prepared in the S2 step into a bearing chamber of the clamp holder, connecting the metal type sample block with the front end face of the rock core chamber behind the clamp holder and coaxially distributing the metal type sample block, then driving an auxiliary pump to operate, adjusting a driving piston to operate, driving the front rock core chamber to operate by the driving piston and clamping and positioning the other end of the metal type sample block, then evacuating the air in the clamp holder through a vacuum pump, enabling the pressure value in the clamp holder to reach-0.19 MPa, and maintaining the pressure for 2-4 hours, thus completing the air tightness detection;
s4, performing experiment prefabrication, taking out the metal type sample block from the clamp holder after the detection operation of the step S3 is completed, installing the coal sample prepared in the step S2 into the clamp holder, evacuating the air in the clamp holder through a vacuum pump again, enabling the pressure value in the clamp holder to reach-0.19 MPa, and maintaining the pressure; then respectively driving a carbon dioxide gas source, a condenser, a high-pressure carbon dioxide pump, a mixer, an extraction kettle, a preheater II, a preheater III, a separation kettle I and a separation kettle II to operate, on one hand, adjusting the operation temperature of the condenser, the mixer, the extraction kettle, the preheater II, the preheater III, the separation kettle I and the separation kettle II to reach the set experimental value in the step S2, on the other hand, driving the high-pressure carbon dioxide pump to operate, pressurizing the carbon dioxide device conveyed by the carbon dioxide gas source, conveying the carbon dioxide into a clamp holder after the temperature and pressure of the condenser and the mixer are adjusted, enabling the air pressure and the temperature in the clamp holder to reach the set experimental value in the step S2, and carrying out subsequent operation after the air pressure and the temperature in the clamp holder reach the set experimental value in the step S2 and carrying out heat preservation and pressure maintenance for 1-3 minutes;
s5, performing an extraction experiment, after the step S4 is completed, communicating a clamp holder with external carbon dioxide gas, disconnecting the clamp holder from an extraction kettle and a preheater II and maintaining pressure, increasing the air pressure in the clamp holder to a set value in the step S2 through an auxiliary pump of a carrying agent pump, a high-pressure carbon dioxide pump and the clamp holder, maintaining the pressure for 96 hours, finally disconnecting the clamp holder from the carbon dioxide gas, taking out a coal sample, naturally cooling the coal sample and the clamp holder to room temperature, weighing and measuring the coal sample on one hand, returning to the step S4 on the other hand, installing a brand new coal sample in the clamp holder, and performing a subsequent experiment;
s6, after the seepage experiment is completed and the step S5 is completed, reading the numerical values of a carbon dioxide flowmeter, a thermometer on a flow guide pipe, a manometer and a thermometer and a manometer at a holder and starting to continuously record; then driving the carrier pump, the high-pressure carbon dioxide pump and the auxiliary pump of the holder to operate, increasing the temperature and the pressure in the holder, firstly increasing the air pressure in the holder to 0.1-0.4 MPa, increasing the temperature to 25-45 ℃, then continuously supplying carbon dioxide gas into the holder, keeping the temperature and the air pressure in the holder to stably operate for 12 hours to achieve adsorption balance, and continuously recording the pressure and the temperature value in the adsorption process; and after the adsorption balance is finished, the pressure value of the carbon dioxide conveyed into the holder is increased to reach 0.4-0.8, the holder is communicated with the extraction kettle and the preheater II, and after the pressure value is kept to stably operate for 5 minutes, data continuous acquisition is started through the pressure and the thermometer, so that the extraction experiment can be finished.
8. The apparatus for supercritical carbon dioxide extraction-permeability testing as claimed in claim 7, wherein: in the step S2, the experimental preset temperature of the condenser is 5 ℃, the conveying pressure of the high-pressure carbon dioxide pump is 10MPa, and the rotating speed is 30 r/min; the critical temperature of the carbon dioxide in the holder is 31.1 ℃, the critical pressure is 7.38 MPa, the experimental temperature is 32 ℃, the extraction pressure is 10MPa, and the experimental time of extraction is set to be 96 hours.
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| CN113607620B (en) * | 2021-07-27 | 2022-08-02 | 东北大学 | Experimental device and method for carbon dioxide directional fracturing and permeability testing |
| CN116590091A (en) * | 2023-05-11 | 2023-08-15 | 山东省葡萄研究院 | Grape seed oil extraction method and extraction device |
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