CN111855377A - Supercritical CO2Test device and method for producing methane by extracting coal coupling biological reaction - Google Patents
Supercritical CO2Test device and method for producing methane by extracting coal coupling biological reaction Download PDFInfo
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- CN111855377A CN111855377A CN202010736561.3A CN202010736561A CN111855377A CN 111855377 A CN111855377 A CN 111855377A CN 202010736561 A CN202010736561 A CN 202010736561A CN 111855377 A CN111855377 A CN 111855377A
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- 239000003245 coal Substances 0.000 title claims abstract description 78
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 50
- 238000010168 coupling process Methods 0.000 title claims abstract description 33
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 33
- 230000008878 coupling Effects 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 137
- 239000007788 liquid Substances 0.000 claims abstract description 93
- 238000000926 separation method Methods 0.000 claims abstract description 80
- 238000003860 storage Methods 0.000 claims abstract description 72
- 238000012360 testing method Methods 0.000 claims abstract description 59
- 238000002347 injection Methods 0.000 claims abstract description 22
- 239000007924 injection Substances 0.000 claims abstract description 22
- 238000011065 in-situ storage Methods 0.000 claims abstract description 17
- 238000004088 simulation Methods 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims description 53
- 229910000831 Steel Inorganic materials 0.000 claims description 23
- 239000010959 steel Substances 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000013060 biological fluid Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 230000000087 stabilizing effect Effects 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 239000011152 fibreglass Substances 0.000 claims description 3
- 230000005484 gravity Effects 0.000 claims description 3
- 239000012263 liquid product Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000010998 test method Methods 0.000 claims description 3
- 235000019580 granularity Nutrition 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 37
- 238000005516 engineering process Methods 0.000 description 7
- 244000005700 microbiome Species 0.000 description 7
- 230000001965 increasing effect Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 3
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- 238000011160 research Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
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- 239000005431 greenhouse gas Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/22—Fuels; Explosives
- G01N33/222—Solid fuels, e.g. coal
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
The invention discloses supercritical CO2A test device and a method for methane production through coal extraction coupling biological reaction are provided. The test device comprises a gas storage device, CO2The device comprises a liquefaction device, an extraction separation device, a biological liquid injection device, an in-situ simulation device and a product collector; the gas storage device is separately connected with CO2The liquefaction device is connected with a biological liquid injection device, and CO2The other end of the liquefaction device is connected with the extraction separation device, the other end of the biological liquid injection device is respectively connected with the extraction separation device and the in-situ simulation device, and the product collector is respectively connected with the extraction separation device and the in-situ simulation device. Supercritical CO utilized in the present invention2Supercritical CO capable of realizing coal crushing by extracting coal coupling biological reaction methane production test device2Extraction coupling generatorA substance reaction methane production test; meanwhile, the supercritical CO of the coal test piece can be developed by simulating the conditions of temperature and pressure of the coal bed2Extraction coupling biological reaction methane production test.
Description
Technical Field
The invention relates to aSupercritical CO2A test device and a method for methane production through extraction coal coupling biological reaction belong to the technical field of microbial enhanced coal bed methane (MECOM).
Background
The energy industry needs to move faster towards low carbon society, which is driving the change in global energy consumption patterns. The exploitation of Coal Bed Methane (CBM) can not only improve the energy supply structure and effectively relieve the energy crisis caused by insufficient fossil energy supply, but also promote the safe exploitation of Coal mines and reduce the emission of greenhouse gases, thereby having great economic, social and environmental significance. However, the development of the coal bed gas industry is severely restricted by the current situation of low coal bed gas recovery ratio. How to realize the yield increase of the coal bed gas becomes important research content of the current coal bed gas development. Among many Coal Bed gas yield increasing technologies, the microorganism Enhanced Coal Bed gas (microbe Enhanced Coal Bed Methane) technology has become a current research hotspot due to the characteristics of being green, free of pollution, capable of generating new Coal Bed gas and the like. Although the technology for increasing the yield of the coal bed gas by microorganisms is proved to be feasible in theory and experiments, the technology is very limited in practical application, the yield increasing effect of the coal bed gas is poor, and the bioavailability is low. Therefore, chemical, physical, biological and other methods must be adopted to improve the conditions for degrading and converting coal by microorganisms, promote the degradation and utilization of the microorganisms, and increase the production of biological coal bed gas. CO22The chemical property is inactive, the product is colorless, tasteless and nontoxic, the safety is good, the supercritical state can be achieved when the temperature is higher than the critical temperature of 31.26 ℃ and the pressure is higher than the critical pressure of 7.4MPa, and the critical condition is easy to achieve. And supercritical CO2The diffusion coefficient is 100 times that of liquid, so that the solvent has extremely strong dissolving capacity. By using the supercritical CO2 as a solvent, organic matters in complex compounds in the coal can be effectively extracted. The technology can be combined with the technology of increasing the yield of coal bed gas by microorganisms, and is favorable for supercritical CO2The free organic matters extracted from the coal can better contact and react with microbial flora, the effective biological substrate concentration in the coal is increased, and the bioavailability is improved. Thus, supercritical CO2Is an effective and feasible method for improving the gas efficiency of the microorganism-enhanced coal bedA method for producing fruit.
Disclosure of Invention
The invention aims to provide supercritical CO2A test device and a method for methane production through coal extraction coupling biological reaction are provided. Supercritical CO capable of crushing coal2Performing an extraction coupling biological reaction methane production test; meanwhile, the supercritical CO of the coal test piece can be developed by simulating the conditions of temperature and pressure of the coal bed2Extraction coupling biological reaction methane production test.
The invention provides supercritical CO2An extraction coal coupling biological reaction methane production test device comprises a gas storage device and CO2The device comprises a liquefaction device, an extraction separation device, a biological liquid injection device, an in-situ simulation device and a product collector; the gas storage device is separately connected with CO2The liquefaction device is connected with a biological liquid injection device, and CO2The other end of the liquefaction device is connected with the extraction separation device, the other end of the biological liquid injection device is respectively connected with the extraction separation device and the in-situ simulation device, and the product collector is respectively connected with the extraction separation device and the in-situ simulation device;
the gas storage device comprises CO2Steel cylinder and N2A steel cylinder; CO22The steel cylinder is connected with a first purifier, N2The steel cylinder is connected with a biological liquid storage tank;
the CO is2The liquefying device comprises a first purifier and CO which are connected in sequence2A storage tank, a plunger pump and a second purifier; the other end of the first purifier is connected with CO2The steel cylinder is connected, and the other end of the second purifier is connected with the extraction kettle;
the extraction separation device comprises an extraction kettle, a first separation kettle and a second separation kettle; one end of an inlet of the extraction kettle is connected with the second purifier through a sixth valve, the other end of the inlet of the extraction kettle is connected with the biological liquid storage tank through a seventeenth valve, an outlet of the extraction kettle is provided with a seventh valve, one end of the inlet of the extraction kettle is connected with the first separation kettle through an eighth valve, the other end of the inlet of the extraction kettle is connected with the holder through an eighteenth valve, a reserved opening in the top of the extraction kettle is connected with the first product collector, the first separation kettle is connected with the second separation kettle, and the second separation kettle is connected with the first purifier through a tenth valve and an eleventh valve to form a circulating;
the biological liquid injection device comprises a water tank, a pressure tracking pump and a biological liquid storage tank; the inlet of the biological liquid storage tank is provided with a thirteenth valve, one end of the thirteenth valve is connected with the pressure tracking pump through a twelfth valve, and the other end of the thirteenth valve is connected with the N through a second valve2The steel cylinder is connected, the outlet of the biological liquid storage tank is provided with a fourteenth valve, one end of the fourteenth valve is connected with the extraction kettle through a seventeenth valve, and the other end of the fourteenth valve is connected with the holder through a fifteenth valve; the pressure tracking pump is connected with the water tank;
the in-situ simulation device comprises a clamp holder, a thermostat and a hand-operated pump; the gripper is arranged in the incubator, one end of the inlet of the gripper is connected with the biological liquid storage tank through a fourteenth valve and a fifteenth valve, the other end of the inlet of the gripper is connected with the extraction kettle through a nineteenth valve, an eighteenth valve and a seventh valve, one end of the outlet of the gripper is connected with the first separation kettle through a sixth valve and a twentieth valve, the other end of the outlet of the gripper is connected with the second product collector, and the hand pump is connected with the gripper to provide axial pressure and confining pressure for the gripper;
the product collector comprises a first product collector and a second product collector and is used for collecting and separating gas-liquid products; the first product collector is connected with the extraction kettle through a twenty-first valve, and the second product collector is connected with the holder through a sixteenth valve.
The device also comprises an automatic pressure stabilizing system, wherein the automatic pressure stabilizing system controls the rotating speed of the plunger pump through the numerical value of a second pressure gauge, automatically adjusts the pressure of the extraction kettle by matching with the opening size of an automatic pressure stabilizing valve, controls the pressure by using a panel switch in a manual mode and an automatic mode, and automatically adjusts the pressure according to the set pressure and the actual pressure of the extraction kettle with the precision of 0.1 MPa.
In the device, the volumes of the extraction kettle, the first separation kettle and the second separation kettle are all 1L, water bath heating is adopted, the highest temperature is not more than 100 ℃, the temperature control precision is 0.1 ℃, and the pressure resistance is 50MPa at most.
In the device, the first product collector and the second product collector are of transverse piston type to eliminate the influence of piston gravity, the device is made of glass fiber reinforced plastic, the highest pressure resistance is 2MPa, a mL scale is attached to the surface of the device to observe the volume of gas and liquid in the device, the first product collector and the second product collector are respectively externally connected with a seventh pressure gauge and an eighth pressure gauge with the accuracy of 0.05MPa and the range of 2MPa, the first product collector is additionally provided with a first air extraction valve for receiving and measuring gas generated by biological reaction, and the second product collector is additionally provided with a second air extraction valve and a first liquid receiving valve for receiving and separating liquid and gas generated by biological reaction.
In the device, the biological liquid storage tank is a piston type storage tank with the volume of 1L, is made of stainless steel and has the highest pressure resistance of 50 MPa.
In the device, the pressure tracking pump is used for injecting the biological liquid into the extraction kettle and the holder, and can adopt 0-10mL/min constant-current injection or 0-20MPa constant-pressure injection, and the precision is 0.0001mL/min and 0.01MPa respectively.
In the device, pipelines, joints and valves used in the whole device are all made of stainless steel materials, the outer diameter of each pipeline is 3mm, the wall thickness is 0.5mm, and the maximum bearable pressure is 50 MPa.
The invention provides supercritical CO2Test method for producing methane by extracting coal coupling biological reaction, and supercritical CO of crushed coal and coal test piece can be realized2Performing an extraction coupling biological reaction methane production test;
supercritical CO of said crushed coal2The extraction and biological reaction system comprises the following specific steps:
(1) placing the prepared biological liquid in a biological liquid storage tank, and then connecting an inlet of the biological liquid storage tank with N through a second valve and a thirteenth valve2The steel bottle is connected, and the outlet of the biological liquid storage tank is connected with the extraction kettle through a fourteenth valve and a seventeenth valve.
(2) Putting coal powder with different granularities into an extraction kettle, and then sealing.
(3) And opening a tenth valve and an eleventh valve, respectively opening heating switches of the extraction kettle, the first separation kettle and the second separation kettle, and heating the equipment to a set test value, wherein the temperature control range is 25-100 ℃.
(4) Opening the first valve and the third valve to make CO2Into CO2In a storage tank for CO2The pressure in the storage tank is more than 4MPa, and the pressure is higher thanOpening the fourth valve, the fifth valve and the sixth valve, and starting the plunger pump to ensure that the pressure in the extraction kettle reaches a set test value, wherein the pressure control range is 0MPa-50 MPa.
(5) And opening the seventh valve and the eighth valve to control the pressure of the first separation kettle to be 0MPa-50MPa after the pressure of the first separation kettle reaches the set test value, and opening the ninth valve to control the pressure of the second separation kettle to reach the set test value, wherein the pressure control range is 0MPa-50 MPa.
(6) When the pressure of the three kettles reaches the set value, the panel valve is adjusted to be automatic, the pressure of the extraction kettle is automatically balanced and maintained, and the crushed coal is extracted.
(7) And respectively collecting extracts of the first separation kettle and the second separation kettle by using a third liquid receiving valve and a fourth liquid receiving valve.
(8) And closing the plunger pump and all valves, opening the first air escape valve to release the pressure in the extraction kettle, and closing the first air escape valve after the pressure of the extraction kettle is reduced to 0 MPa.
(9) Opening the second, thirteenth, fourteenth and seventeenth valves using N2The biological liquid is injected into the extraction kettle quickly by air pressure, and the twenty-first valve is opened to carry out biological reaction.
(10) The second liquid receiving valve is used for collecting reaction liquid, the first product collector is used for collecting gas, and the generated gas is measured by an injector at the first air suction valve.
Supercritical CO of the coal test piece2The extraction and biological reaction system comprises the following specific steps:
(1) and (3) placing the prepared biological liquid into a biological liquid storage tank, wherein the inlet of the biological liquid storage tank is connected with a pressure tracking pump through a twelfth valve and a thirteenth valve, and the outlet of the biological liquid storage tank is connected with a holder through a fourteenth valve and a fifteenth valve.
(2) The coal test piece is placed into a holder and then sealed by a plug.
(3) A hand-operated pump is used for providing test set axial pressure and test set confining pressure for the clamp holder, and a thermostat is used for heating the clamp holder to a set temperature, wherein the temperature control range is 25-100 ℃.
(4) And opening a tenth valve and an eleventh valve, respectively opening heating switches of the extraction kettle 7, the first separation kettle 8 and the second separation kettle 9, and heating the equipment to a set test value, wherein the temperature control range is 25-100 ℃.
(5) Opening the first valve and the third valve to make CO2Into CO2In a storage tank for CO2The pressure in the storage tank is more than 4MPa, the fourth valve, the fifth valve and the sixth valve are controlled, and the plunger pump is started to ensure that the pressure in the extraction kettle reaches a set test value, and the pressure control range is 0MPa-50 MPa.
(6) And opening a seventh valve, an eighteenth valve, a nineteenth valve, a sixth valve, a twentieth valve and a ninth valve to extract the coal test piece, and collecting the extracts of the first separation kettle and the second separation kettle by using a third liquid receiving valve and a fourth liquid receiving valve respectively.
(7) And closing the plunger pump and all valves, opening the first air escape valve to release the pressure in the extraction kettle, and closing the first air escape valve after the pressure of the extraction kettle is reduced to 0 MPa.
(8) And opening the twelfth valve, the thirteenth valve, the fourteenth valve, the fifteenth valve and the sixteenth valve, starting the pressure tracking pump, gradually injecting the biological fluid into the holder in a constant-current or constant-pressure mode, and carrying out biological reaction.
(9) And separating the biological reaction liquid and the generated gas by using a second product collector, collecting the liquid by using a first liquid receiving valve, and measuring the generated gas by using an injector at a second gas extraction valve.
The invention has the beneficial effects that:
(1) the supercritical CO2The extraction coal coupling biological reaction methane production test device can provide CO under different temperature and pressure conditions2Reaching supercritical state, and using supercritical CO2Extracting the crushed coal, directly carrying out biological reaction on the extracted coal, and receiving the product.
(2) The supercritical CO2The extraction coal coupling biological reaction methane production test device can provide axial pressure confining pressure to simulate an in-situ test and utilize supercritical CO2The extraction of the coal test piece is carried out,and injecting biological fluid into the clamp holder to carry out biological reaction on the coal test piece.
(3) The invention not only provides a technology for increasing the yield of coal bed gas by microorganisms and supercritical CO2The combination of the extraction technology provides a brand new device, and provides a feasible method for exploiting the coal bed gas under the simulated in-situ condition.
Drawings
FIG. 1 is a schematic view of the structure of the test apparatus of the present invention.
In the figure: 1 is CO2Steel cylinder, 2 is N2A steel cylinder, 3 is a first purifier, 4 is CO2A storage tank, 5 is a plunger pump, 6 is a second purifier, 7 is an extraction tank, 8 is a first separation tank, 9 is a second separation tank, 10 is a water tank, 11 is a pressure tracking pump, 12 is a biological fluid storage tank, 13 is a holder, 14 is a first product collector, 15 is a second product collector, 16 is a first flow meter, 17 is a second flow meter, 18 is a first valve, 19 is a second valve, 20 is a third valve, 21 is a fourth valve, 22 is a fifth valve, 23 is a sixth valve, 24 is a seventh valve, 25 is an eighth valve, 26 is a ninth valve, 27 is a tenth valve, 28 is an eleventh valve, 29 is a twelfth valve, 30 is a thirteenth valve, 31 is a fourteenth valve, 32 is a fifteenth valve, 33 is a sixteenth valve, 34 is a first suction valve, 35 is a first liquid receiving valve, 36 is a seventeenth valve, 37 is an eighteenth valve, 38 is a nineteenth valve, 39 is a twentieth valve, 40 is a first air release valve, 41 is a second air release valve, 42 is a third air release valve, 43 is a second liquid receiving valve, 44 is a third liquid receiving valve, 45 is a fourth liquid receiving valve, 46 is a second air suction valve, 47 is an automatic pressure stabilizing valve, 48 is a first pressure gauge, 49 is a second pressure gauge, 50 is a third pressure gauge, 51 is a fourth pressure gauge, 52 is a fifth pressure gauge, 53 is a sixth pressure gauge, 54 is a first temperature gauge, 55 is a second temperature gauge, 56 is a third temperature gauge, 57 is a fourth temperature gauge, 58 is a seventh pressure gauge, 59 is an eighth pressure gauge, 60 is a hand pump, 61 is a twenty-first valve, and 62 is a constant temperature box.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
As shown in FIG. 1, a supercritical CO2The device for extracting methane by coal coupling biological reaction comprises a gas storage device and CO2The device comprises a liquefaction device, an extraction separation device, a biological liquid injection device, an in-situ simulation device and a product collector; the gas storage device is separately connected with CO2The liquefaction device is connected with a biological liquid injection device, and CO2The other end of the liquefaction device is connected with the extraction separation device, the other end of the biological liquid injection device is respectively connected with the extraction separation device and the in-situ simulation device, and the product collector is respectively connected with the extraction separation device and the in-situ simulation device;
the gas storage device comprises CO2Steel cylinders 1 and N2A steel cylinder 2; CO22The steel cylinder 1 is connected with a first purifier 3, N2The steel cylinder 2 is connected with a biological liquid storage tank 12;
the CO is2The liquefying device comprises a first purifier 3 and CO which are connected in sequence2A storage tank 4, a plunger pump 5 and a second purifier 6; the other end of the first purifier 3 is connected with CO2The steel cylinder 1 is connected, and the other end of the second purifier 6 is connected with the extraction kettle 7;
the extraction separation device comprises an extraction kettle 7, a first separation kettle 8 and a second separation kettle 9; one end of an inlet of the extraction kettle 7 is connected with the second purifier 6 through a sixth valve 23, the other end of the inlet of the extraction kettle 7 is connected with the biological liquid storage tank 12 through a seventeenth valve 36, an outlet of the extraction kettle 7 is provided with a seventh valve 24, one end of the seventh valve 24 is connected with the first separation kettle 8 through an eighth valve 25, the other end of the seventh valve is connected with the holder 13 through an eighteenth valve 37, a reserved opening at the top of the extraction kettle 7 is connected with the first product collector 14, the first separation kettle 8 is connected with the second separation kettle 9, and the second separation kettle 9 is connected with the first purifier 3 through a tenth valve 27 and an eleventh valve 28 to form a circulating system;
the biological liquid injection device comprises a water tank 10, a pressure tracking pump 11 and a biological liquid storage tank 12; the inlet of the biological liquid storage tank 12 is provided with a thirteenth valve 30, one end of the thirteenth valve is connected with the pressure tracking pump 11 through a twelfth valve 29, and the other end of the thirteenth valve is connected with N through a second valve 192The steel cylinder 2 is connected, the outlet of the biological liquid storage tank 12 is provided with a fourteenth valve 31, one end of the fourteenth valve is connected with the extraction kettle 7 through a seventeenth valve 36, and the other end is connected with the extraction kettle 7The end is connected with the clamper 13 through a fifteenth valve 32; the pressure tracking pump 11 is connected with the water tank 10;
the in-situ simulation device comprises a clamp holder 13, a constant temperature box 62 and a hand pump 60; the clamp 13 is arranged in the incubator 62, one end of the inlet of the clamp 13 is connected with the biological liquid storage tank 12 through a fourteenth valve 31 and a fifteenth valve 32, the other end of the inlet of the clamp 13 is connected with the extraction kettle 7 through a nineteenth valve 38, an eighteenth valve 37 and a seventh valve 24, one end of the outlet of the clamp 13 is connected with the first separation kettle 8 through a sixth valve 23 and a twentieth valve 39, the other end of the outlet of the clamp is connected with the second product collector 15, and the hand pump 60 is connected with the clamp 13 to provide axial pressure and confining pressure for the clamp 13;
the product collector comprises a first product collector 14 and a second product collector 15, and is used for collecting and separating gas-liquid products; the first product collector 14 is connected to the extraction vessel 7 via a twenty-first valve 61, and the second product collector 15 is connected to the holder 13 via a sixteenth valve 33.
In the device, the automatic pressure stabilizing system is further included, the rotating speed of the plunger pump 5 is controlled by the numerical value of the second pressure gauge 49, the pressure of the extraction kettle 7 is automatically adjusted by matching with the opening of the automatic pressure stabilizing valve 47, the manual and automatic control is realized by using a panel switch, the automatic adjustment is realized according to the set pressure and the actual pressure of the extraction kettle 7, and the precision is 0.1 MPa.
In the device, the volumes of the extraction kettle 7, the first separation kettle 8 and the second separation kettle 9 are all 1L, water bath heating is adopted, the highest temperature is not more than 100 ℃, the temperature control precision is 0.1 ℃, and the pressure resistance can be 50MPa at most.
In the device, the first product collector 14 and the second product collector 15 are horizontal piston type to eliminate the gravity effect of the piston, the device is made of glass fiber reinforced plastic, the highest pressure resistance is 2MPa, the surface is provided with a mL scale to observe the volume of gas and liquid in the device, the first product collector 14 is externally connected with a seventh pressure gauge 58 with the precision of 0.05MPa and the range of 2MPa, a first air suction valve 34 is arranged to receive and measure the gas generated by the biological reaction, the second product collector 15 is externally connected with an eighth pressure gauge 59 with the precision of 0.05MPa and the range of 2MPa, and a second air suction valve 46 and a first liquid receiving valve 35 are arranged to receive and separate the liquid and the gas generated by the biological reaction.
In the above device, the biological liquid storage tank 12 is a piston type storage tank with a volume of 1L, is made of stainless steel, and has a maximum pressure resistance of 50 MPa.
In the device, a pressure tracking pump 11 is used for injecting the biological liquid into the extraction kettle 7 and the holder 13, and the constant-current injection of 0-10mL/min or the constant-pressure injection of 0-20MPa is selected, and the precision is 0.0001mL/min and 0.01MPa respectively.
In the device, the pipeline, the joint and the valve used in the whole device are all made of stainless steel, the outer diameter of the pipeline is 3mm, the wall thickness is 0.5mm, and the maximum bearable pressure is 50 MPa.
The test device provided by the invention can realize supercritical CO of crushed coal2Performing an extraction coupling biological reaction methane production test; meanwhile, the supercritical CO of the coal test piece can be developed by simulating the conditions of temperature and pressure of the coal bed2Extraction coupling biological reaction methane production test. The following examples are intended to illustrate the present invention.
Example 1: supercritical CO2Coupling biological reaction of extracted coal powder
(1) Placing the prepared 1L of biological fluid in the biological fluid storage tank 12, and then connecting the inlet of the biological fluid storage tank 12 with N through the second valve 19 and the thirteenth valve 302The steel cylinder 2 is connected, and the outlet of the biological liquid storage tank 7 is connected with the extraction kettle 7 through a fourteenth valve 31 and a seventeenth valve 36.
(2) 60-80 mesh coal powder is put into the extraction kettle 7 and then sealed.
(3) The tenth valve 27 and the eleventh valve 28 are opened, and the heating switches of the extraction kettle 7, the first separation kettle 8 and the second separation kettle 9 are opened respectively to heat to 35 ℃, 30 ℃ and 25 ℃.
(4) Opening the first valve 18 and the third valve 20 to allow CO2Into CO2In a storage tank 4, waiting for CO2The pressure in the storage tank 4 reaches 4.5MPa, the fourth valve 21, the fifth valve 22 and the sixth valve 23 are opened, and the plunger pump 5 is started, so that the pressure in the extraction kettle 7 reaches 10 MPa.
(5) The seventh valve 24 and the eighth valve 25 are opened to make the pressure of the first separation kettle 8 reach 8MPa, and the ninth valve 26 is opened to make the pressure of the second separation kettle 9 reach 7 MPa.
(6) When the pressure of the three kettles reaches a set value, the panel valve is adjusted to be automatic, the pressure of the extraction kettle 7 is automatically balanced and maintained, and the crushed coal is extracted for 4 hours;
(7) respectively collecting extracts of the first separation kettle 8 and the second separation kettle 9 by using a third liquid receiving valve 44 and a fourth liquid receiving valve 45;
(8) closing the plunger pump 5 and all valves, opening the first air escape valve 40 to release the pressure in the extraction kettle, and closing the first air escape valve 40 after the pressure of the extraction kettle 7 is reduced to 0 MPa;
(9) opening the second, thirteenth, fourteenth and seventeenth valves 19, 30, 31, 36 with N2The biological liquid is quickly injected into the extraction kettle 7 by air pressure, and the twenty-first valve 61 is opened to carry out biological reaction;
(10) the second liquid receiving valve 43 is used for collecting the reaction liquid, the first product collector 14 is used for collecting the gas, and the gas generated is measured by an injector at the first gas extraction valve 34.
Example 2: supercritical CO2Coupling biological reaction of extracted coal test piece
(1) The prepared 1L of biological fluid is placed in the biological fluid storage tank 12, the inlet of the biological fluid storage tank 12 is connected with the pressure tracking pump 11 through the twelfth valve 29 and the thirteenth valve 30, and the outlet of the biological fluid storage tank 12 is connected with the clamper 13 through the fourteenth valve 31 and the fifteenth valve 32.
(2) A coal specimen having a size of phi 25X 50mm was placed in the holder 13 and then sealed with a plug.
(3) The holder 13 was subjected to a test of 10MPa axial pressure and 10MPa confining pressure using a hand pump 60, and heated to 35 ℃ using a thermostat 62.
(4) The tenth valve 27 and the eleventh valve 28 are opened, and the heating switches of the extraction kettle 7, the first separation kettle 8 and the second separation kettle 9 are opened respectively to heat to 35 ℃, 30 ℃ and 25 ℃.
(5) Opening the first valve 18 and the third valve 20 to allow CO2Into CO2In the storage tank 4, the water is stored,to be treated with CO2The pressure in the storage tank 4 reaches 4.5MPa, the fourth valve 21, the fifth valve 22 and the sixth valve 23 are controlled, and the plunger pump 5 is started to ensure that the pressure in the extraction kettle 7 reaches 10 MPa.
(6) And opening the seventh valve 24, the eighteenth valve 37, the nineteenth valve 38, the sixth valve 23, the twentieth valve 39 and the ninth valve 26, extracting the coal sample for 4 hours, and collecting the extracts of the first separation kettle 8 and the second separation kettle 9 by using the third liquid receiving valve 44 and the fourth liquid receiving valve 45 respectively.
(7) And closing the plunger pump 5 and all valves, opening the first air release valve 40 to release the pressure in the extraction kettle 7, and closing the first air release valve 40 after the pressure of the extraction kettle 7 is reduced to 0 MPa.
(8) The twelfth valve 29, the thirteenth valve 30, the fourteenth valve 31, the fifteenth valve 32, and the sixteenth valve 33 are opened, the pressure-tracking pump 11 is started, and the biological fluid is injected into the holder 13 at a constant pressure of 7MPa to perform a biological reaction.
(9) The biological reaction solution and the generated gas are separated by the second product trap 15, the solution is collected by the first solution receiving valve 35, and the generated gas is measured by the syringe at the second gas extraction valve 46.
Claims (9)
1. Supercritical CO2Test device of methane is produced in extraction coal coupling biological reaction, its characterized in that: comprising a gas storage means, CO2The device comprises a liquefaction device, an extraction separation device, a biological liquid injection device, an in-situ simulation device and a product collector; the gas storage device is separately connected with CO2The liquefaction device is connected with a biological liquid injection device, and CO2The other end of the liquefaction device is connected with the extraction separation device, the other end of the biological liquid injection device is respectively connected with the extraction separation device and the in-situ simulation device, and the product collector is respectively connected with the extraction separation device and the in-situ simulation device;
the gas storage device comprises CO2Steel cylinder and N2A steel cylinder; CO22Steel cylinder and CO2The liquefaction plant is connected, N2The steel cylinder is connected with the biological liquid injection device;
the CO is2The liquefaction plant comprisesConnected first purifier, CO2A storage tank, a plunger pump and a second purifier; the first purifier is connected with CO through a third valve2Storage tank connected to CO2The storage tank is connected with the plunger pump through a fourth valve, and the plunger pump is connected with the second purifier through a fifth valve; CO22The steel cylinder is connected with the first purifier; the extraction kettle is connected with a second purifier;
the extraction separation device comprises an extraction kettle, a first separation kettle and a second separation kettle; the extraction kettle is connected with the first separation kettle through a seventh valve and an eighth valve, and the first separation kettle is connected with the second separation kettle through a ninth valve; one end of the inlet of the extraction kettle is connected with the second purifier through a sixth valve, and the other end of the inlet of the extraction kettle is connected with the biological liquid storage tank through a seventeenth valve; the holder is connected with the outlet of the extraction kettle; the first product collector is connected with a reserved opening at the top of the extraction kettle; the first purifier is connected with the second separation kettle to form a circulating system;
the biological liquid injection device comprises a water tank, a pressure tracking pump and a biological liquid storage tank; the water tank is connected with a pressure tracking pump, and the pressure tracking pump is connected with the biological liquid storage tank through a twelfth valve and a thirteenth valve; a fourteenth valve is arranged at the outlet of the biological liquid storage tank, one end of the fourteenth valve is connected with the extraction kettle through a seventeenth valve, and the other end of the fourteenth valve is connected with the holder through a fifteenth valve; n is a radical of2The steel cylinder is connected with the inlet of the biological liquid storage tank;
the in-situ simulation device comprises a clamp holder, a thermostat and a hand-operated pump; the holder is arranged in the incubator, and the hand-operated pump is connected with the holder to provide axial pressure and confining pressure for the holder; one end of the inlet of the holder is connected with the biological liquid storage tank through a fourteenth valve and a fifteenth valve, and the other end of the inlet of the holder is connected with the extraction kettle through a nineteenth valve, an eighteenth valve and a seventh valve; one end of the outlet of the gripper is connected with the first separation kettle through a sixth valve and a twentieth valve, the other end is connected with the second product collector through a sixteenth valve,
the product collector comprises a first product collector and a second product collector and is used for collecting and separating gas-liquid products; the first product collector is connected with the extraction kettle through a twenty-first valve; the second product collector is connected to the holder via a sixteenth valve.
2. The supercritical CO of claim 12Test device of methane is produced in extraction coal coupling biological reaction, its characterized in that: the automatic pressure stabilizing system controls the rotating speed of the plunger pump through the numerical value of a second pressure gauge, automatically adjusts the pressure of the extraction kettle by matching with the opening size of an automatic pressure stabilizing valve, controls the pressure manually and automatically by using a panel switch, and automatically adjusts the pressure according to the set pressure and the actual pressure of the extraction kettle with the precision of 0.1 MPa.
3. The supercritical CO of claim 12Test device of methane is produced in extraction coal coupling biological reaction, its characterized in that: the volumes of the extraction kettle, the first separation kettle and the second separation kettle are all 1L, water bath heating is adopted, the highest temperature is not more than 100 ℃, the temperature control precision is 0.1 ℃, and the pressure resistance can be 50MPa at most.
4. The supercritical CO of claim 12Test device of methane is produced in extraction coal coupling biological reaction, its characterized in that: the first product collector and the second product collector are of transverse piston type to eliminate the influence of piston gravity, are made of glass fiber reinforced plastic materials, have the highest pressure resistance of 2MPa, and are provided with mL scales on the surfaces to observe the volume of gas and liquid in the inner part; the first product collector and the second product collector are respectively and externally connected with a seventh pressure gauge and an eighth pressure gauge with the accuracy of 0.05MPa and the range of 2MPa, the first product collector is provided with a first air extraction valve for receiving and measuring gas generated by biological reaction, and the second product collector is provided with a second air extraction valve and a first liquid receiving valve for receiving and separating liquid and gas generated by biological reaction.
5. The supercritical CO of claim 12Test device of methane is produced in extraction coal coupling biological reaction, its characterized in that: the biological liquid storage tank adopts a piston type storage tank with the volume of 1L, adopts stainless steel materials and has the highest pressure resistance of 50 MPa.
6. The supercritical CO of claim 12Test device of methane is produced in extraction coal coupling biological reaction, its characterized in that: the pressure tracking pump is used for injecting the biological liquid into the extraction kettle and the holder, and the constant-current injection of 0-10mL/min or the constant-pressure injection of 0-20MPa is selected, and the precision is 0.0001mL/min and 0.01MPa respectively.
7. The supercritical CO of claim 12Test device of methane is produced in extraction coal coupling biological reaction, its characterized in that: the pipeline, the joint and the valve used in the whole device are all made of stainless steel, the outer diameter of the pipeline is 3mm, the wall thickness is 0.5mm, and the maximum bearable pressure is 50 MPa.
8. Supercritical CO2A test method for methane production by extraction coal coupling biological reaction, which adopts the supercritical CO of any one of claims 1-72Test device of methane is produced in extraction coal coupling biological reaction, its characterized in that: supercritical CO with crushed coal as treatment object2Performing an extraction coupling biological reaction methane production test; the specific implementation steps are as follows:
(1) placing the prepared biological liquid in a biological liquid storage tank, and then connecting an inlet of the biological liquid storage tank with N through a second valve and a thirteenth valve2The steel cylinder is connected, and the outlet of the biological liquid storage tank is connected with the extraction kettle through a fourteenth valve and a seventeenth valve;
(2) putting coal powder with different granularities into an extraction kettle, and then sealing;
(3) opening a tenth valve and an eleventh valve, respectively opening heating switches of the extraction kettle, the first separation kettle and the second separation kettle, and heating the equipment to a set test value, wherein the temperature control range is 25-100 ℃;
(4) opening the first valve and the third valve to make CO2Into CO2In a storage tank for CO2Opening a fourth valve, a fifth valve and a sixth valve when the pressure in the storage tank is more than 4MPa, and starting a plunger pump to enable the pressure in the extraction kettle to reach a set test value, wherein the pressure control range is 0MPa-50 MPa;
(5) opening the seventh valve and the eighth valve to control the pressure of the first separation kettle to be 0MPa-50MPa after the pressure of the first separation kettle reaches a set test value, and opening the ninth valve to control the pressure of the second separation kettle to reach the set test value, wherein the pressure control range is 0MPa-50 MPa;
(6) when the pressure of the three kettles reaches a set value, the panel valve is adjusted to be automatic, the pressure of the extraction kettle is automatically balanced and maintained, and the crushed coal is extracted;
(7) respectively collecting extracts of the first separation kettle and the second separation kettle by using a third liquid receiving valve and a fourth liquid receiving valve;
(8) closing the plunger pump and all valves, opening the first air escape valve to release the pressure in the extraction kettle, and closing the first air escape valve after the pressure of the extraction kettle is reduced to 0 MPa;
(9) opening the second, thirteenth, fourteenth and seventeenth valves using N2Quickly injecting the biological liquid into the extraction kettle by air pressure, and opening the twenty-first valve to perform biological reaction;
(10) the second liquid receiving valve is used for collecting reaction liquid, the first product collector is used for collecting gas, and the generated gas is measured by an injector at the first air suction valve.
9. Supercritical CO2A test method for methane production by extraction coal coupling biological reaction, which adopts the supercritical CO of any one of claims 1-72Test device of methane is produced in extraction coal coupling biological reaction, its characterized in that: simulating the conditions of temperature and pressure of the coal bed to develop the supercritical CO of the coal test piece2The extraction coupling biological reaction methane production test comprises the following specific steps:
(1) placing the prepared biological liquid in a biological liquid storage tank, wherein the inlet of the biological liquid storage tank is connected with a pressure tracking pump through a twelfth valve and a thirteenth valve, and the outlet of the biological liquid storage tank is connected with a holder through a fourteenth valve and a fifteenth valve;
(2) putting the coal test piece into a holder, and then sealing by using a plug;
(3) providing a test set axial pressure and a test set confining pressure for the clamp holder by using a hand-operated pump, and heating the clamp holder to a set temperature by using a constant temperature box, wherein the temperature control range is 25-100 ℃;
(4) opening a tenth valve and an eleventh valve, respectively opening heating switches of the extraction kettle, the first separation kettle and the second separation kettle, and heating the equipment to a set test value, wherein the temperature control range is 25-100 ℃;
(5) opening the first valve and the third valve to make CO2Into CO2In a storage tank for CO2The pressure in the storage tank is more than 4MPa, the fourth valve, the fifth valve and the sixth valve are arranged, and the plunger pump is started, so that the pressure in the extraction kettle reaches a set test value, and the pressure control range is 0MPa-50 MPa;
(6) opening a seventh valve, an eighteenth valve, a nineteenth valve, a sixth valve, a twentieth valve and a ninth valve, extracting the coal test piece, and collecting the extracts of the first separation kettle and the second separation kettle by using a third liquid receiving valve and a fourth liquid receiving valve respectively;
(7) closing the plunger pump and all valves, opening the first air escape valve to release the pressure in the extraction kettle, and closing the first air escape valve after the pressure of the extraction kettle is reduced to 0 MPa;
(8) opening a twelfth valve, a thirteenth valve, a fourteenth valve, a fifteenth valve and a sixteenth valve, starting a pressure tracking pump, gradually injecting the biological fluid into the holder in a constant-current or constant-pressure mode, and carrying out biological reaction;
(9) and separating the biological reaction liquid and the generated gas by using a second product collector, collecting the liquid by using a first liquid receiving valve, and measuring the generated gas by using an injector at a second gas extraction valve.
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