Device and method for testing negative carbon quantity in whole process of sealing carbon dioxide by filling body

Abstract

The invention discloses a device and a method for testing the negative carbon amount in the whole process of sealing carbon dioxide by a filling body. The device comprises a filling body sealing carbonization subsystem, a high-pressure gas injection subsystem, a triaxial stress loading subsystem, a constant-temperature control subsystem, a data acquisition subsystem and a vacuumizing subsystem. The stress loading subsystem and the constant temperature control subsystem are used for simulating real filling and sealing conditions, helium and carbon dioxide are injected through the high-pressure gas injection subsystem, and the high-pressure gas injection subsystem is used for measuring the free space volume of the reaction kettle and the negative carbon amount and permeability of a filling body. According to the invention, the problem that the sealing capacity and the sealing efficiency are difficult to accurately measure in the existing simulation test for sealing carbon dioxide by the filling body is solved, and the whole-process simulation test for sealing carbon dioxide by the filling body under triaxial stress loading, temperature control and gas injection pressure control can be realized; the negative carbon amount and the permeability of the filling body in the whole sealing process can be accurately tested, and experimental support is provided for research of a carbon dioxide sealing mechanism of the filling body and technical field application thereof.

Description

Technical Field

[0001] The present invention relates to the technical field of underground carbon dioxide storage, and in particular to a device and method for testing the negative carbon content of a filling body during the whole process of carbon dioxide storage. Background Art

[0002] The production and combustion of fossil fuels such as coal will produce a large amount of carbon dioxide and pollutant gases, which is one of the main sources of carbon emissions. In addition, the production of coal-based solid wastes such as coal gangue and fly ash produced during coal mining and utilization is huge, which will further cause ecological and environmental pollution if not properly handled. How to achieve large-scale disposal of coal-based solid wastes while sealing carbon dioxide is a key problem in the low-carbon green development of coal.

[0003] During the process of CO2 flowing and migrating in the filling body, it constantly contacts the pore surface of the filling body, undergoing physical and chemical reactions such as adsorption, dissolution, and mineralization, so that CO2 can be stably sealed inside the filling body. It is crucial to clarify the sealing capacity and sealing efficiency of the filling body for the on-site application of the filling and sealing CO2 technology. The mine ground stress environment and the physical parameters of the filling body can directly affect the porosity and permeability characteristics of the filling body, thereby causing changes in the sealing capacity and sealing efficiency of the filling body. Therefore, the filling and sealing capacity and stability evaluation of CO2 must consider the stress state of the filling body. In addition, the injection pressure and formation temperature of CO2 will cause changes in the thermodynamic properties of CO2, which in turn affects the sealing capacity and sealing efficiency of the filling body. Therefore, it is necessary to study the sealing law of the filling body under triaxial stress conditions, but the existing device only considers the adsorption of coal and rock, and cannot realize the long-term simulation test of the filling body sealing CO2 under triaxial stress conditions, and cannot accurately calculate the negative carbon content and permeability of the filling body during the whole process of CO2 sealing. Summary of the invention

[0004] Technical problem to be solved: In view of the problem that the storage capacity and storage efficiency of carbon dioxide stored in coal and rock in the prior art are difficult to be accurately and long-term measured, the present invention proposes a device and method for testing the negative carbon content of a filling body during the whole process of carbon dioxide storage. The device adopts a stress loading subsystem and a constant temperature control subsystem to simulate the mine filling and storage environment, and injects helium and carbon dioxide in sequence through a high-pressure gas injection subsystem to measure the free space volume of the reactor and the negative carbon content and permeability of the filling body. The method of the present invention can accurately monitor the negative carbon content and permeability of the filling body during the whole process of carbon dioxide storage, and obtain the change pattern of the negative carbon content of the filling body over time, which is used to analyze the mechanism of filling and storing carbon dioxide.

[0005] Technical solution: One of the purposes of the present invention is to provide a filling body carbonization test device for the whole process of carbon dioxide storage, the test device comprises: a filling body carbonization subsystem, a high-pressure gas injection subsystem, a triaxial stress loading subsystem, a constant temperature control subsystem, a vacuum pumping subsystem and a data acquisition subsystem.

[0006] The main structure of the filling body sealing carbonization subsystem is a reactor, which is a horizontal triaxial core holder in which the rock sample is replaced by the filling body sample, including a confining pressure structure arranged around the filling body sample, an axial pressure structure arranged at one end of the filling body sample, and horizontal air inlets and air outlets arranged at both ends of the filling body sample, a confining pressure inlet is provided on the confining pressure structure, and an axial pressure inlet is provided on the axial pressure structure;

[0007] The high-pressure gas injection subsystem includes a standard chamber, a CO2 boosting pipeline and a He boosting pipeline. The CO2 boosting pipeline includes a high-pressure CO2 storage tank, and the He boosting pipeline includes a high-pressure He storage tank. One end of the standard chamber is connected to the high-pressure CO2 storage tank and the high-pressure He storage tank pipeline respectively, and the other end is connected to the air inlet of the reactor. A valve c and a pressure sensor a are provided at the outlet of the high-pressure CO2 storage tank, a valve d and a pressure sensor b are provided at the outlet of the high-pressure He storage tank, a valve e and a pressure sensor c are provided at the outlet of the standard chamber, and a valve f and a pressure sensor d are provided at the air inlet of the reactor;

[0008] The triaxial stress loading subsystem includes an axial pressure pump and a confining pressure pump, which are respectively connected to the confining pressure inlet and the axial pressure inlet pipeline;

[0009] The constant temperature control subsystem includes a constant temperature water bath and a temperature sensor connected thereto, wherein the constant temperature water bath is arranged outside the reaction kettle and the standard chamber and is used to adjust the temperature;

[0010] The vacuum pumping subsystem includes a vacuum pump, which is connected to the air outlet of the reactor. A pressure sensor f is provided at the inlet of the vacuum pump, and a pressure sensor e and a valve g are provided at the air outlet of the reactor in sequence.

[0011] The data acquisition subsystem includes a data acquisition unit and a data analysis unit. The data acquisition unit includes pressure sensor a, pressure sensor b, pressure sensor c, pressure sensor d, pressure sensor e, pressure sensor f and a temperature sensor. The data analysis unit is a controller and a display. The input end of the controller is electrically connected to the pressure sensor a, pressure sensor b, pressure sensor c, pressure sensor d, pressure sensor e, pressure sensor f and the temperature sensor, respectively, and the output end is electrically connected to the display.

[0012] Preferably, the negative carbon content testing device for the whole process of carbon dioxide sealing by the filling body also includes a seepage monitoring subsystem, which includes a condenser, a saturated sodium bicarbonate solution storage tank, and an electronic balance connected in sequence by pipelines, the air inlet end of the condenser is connected to the air outlet pipe of the reactor, a valve j and a gas flow sensor are provided at the air inlet end of the condenser, the electronic balance is used to weigh the mass of the solution discharged from the saturated sodium bicarbonate solution storage tank, and the gas flow sensor and the electronic balance are electrically connected to the input end of the controller respectively.

[0013] Preferably, the CO2 boosting pipeline also includes a CO2 gas cylinder, a boosting pump a, and an air compressor a. The CO2 gas cylinder, a valve a, a boosting pump a, a pressure sensor a, a valve c and a high-pressure CO2 storage tank are connected in sequence by pipelines, the pipeline between the pressure sensor a and the valve c is connected to the standard chamber, and the air compressor a is connected to the boosting pump a to provide gas pressure; the He boosting pipeline also includes a He gas cylinder, a boosting pump b, and an air compressor b. The He gas cylinder, a valve b, a boosting pump b, a pressure sensor b, a valve d and a high-pressure He storage tank are connected in sequence by pipelines, the pipeline between the pressure sensor b and the valve d is connected to the standard chamber, and the air compressor and the boosting pump b are connected to provide gas pressure.

[0014] Preferably, the reactor comprises a reactor cylinder, a piston, a plug, a first clamping cap, a second clamping cap, a first fixing ring, a second fixing ring, and a rubber sleeve. The rubber sleeve is axially arranged inside the reactor cylinder. The rubber sleeve has a cavity that accommodates the filling body sample to be tested and passes through axially. The first clamping cap and the second clamping cap are respectively embedded around the piston and the plug and are arranged at both ends of the reactor cylinder. The first fixing ring and the second fixing ring are respectively arranged at both ends of the rubber sleeve and are respectively pressed against the inner ends of the first clamping cap and the second clamping cap. The piston passes through the first clamping cap and is arranged at The first fixed sleeve is hollow inside and can move left and right inside the cavity. The plug passes through the second clamping cap and is arranged inside the second fixed sleeve, and the inner end of the plug is pressed against the side end of the filling body sample. The axial center opening of the piston and the plug forms horizontal air inlet and air outlet holes for air inlet and outlet at both ends of the filling body sample. The outer wall of the rubber sleeve, the inner wall of the reactor cylinder and the first fixed sleeve and the second fixed sleeve at both ends form a confining pressure cavity, and the confining pressure inlet is arranged on the reactor cylinder. The cavity formed by the piston, the first clamping cap and the first fixed sleeve is an axial pressure cavity, and the axial pressure inlet is arranged on the first clamping cap.

[0015] Preferably, the reactor further comprises a bracket, which is arranged at the bottom of the reactor and is used to support the reactor.

[0016] Preferably, the vacuum pumping subsystem further comprises a buffer device, which is arranged between the pipeline connected to the pressure sensor f and the valve g, and a valve h is provided at the inlet of the buffer device, a valve i is provided at one outlet, and the other outlet is connected to the pipeline of the pressure sensor f.

[0017] Another object of the present invention is to provide a method for testing the negative carbon content of a filling body during the whole process of carbon dioxide storage based on the above-mentioned negative carbon content testing device for the whole process of carbon dioxide storage by a filling body, the steps of which are as follows:

[0018] Step 1: Place the filling body sample into a reactor, and connect the filling body to a negative carbon content test device for the whole process of carbon dioxide sealing;

[0019] Step 2: Close all valves, open valve d and valve e, inject He into the standard chamber, and then open valve f to perform air tightness test of the device;

[0020] Step 3: Close all valves, open valve e, valve f, valve g, and turn on the vacuum pump to establish the vacuum of the device;

[0021] Step 4: Set the temperature of the constant temperature water bath and apply axial pressure and confining pressure through the triaxial stress loading subsystem;

[0022] Step 5: Close all valves, open valve d and valve e, inject He into the standard chamber, close valve d, and wait until the pressure sensor c indicates a stable reading of P. S1 After that, open valve f. When the readings of pressure sensor c and pressure sensor d are the same and stable at P R2 When the free space volume of the device is calculated, the calculation formula is as follows:

[0023]

[0024] Where V R is the volume of the standard chamber, cm 3 ; V S is the pore volume of the reactor filling, cm 3 ;P S1 is the initial He pressure in the standard chamber, MPa; P R2 is the He pressure in the reactor after stabilization, MPa; Z S1 , Z R2 They are the compression factor of the initial He in the standard chamber and the compression factor of the stabilized He in the reactor, respectively, which are obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States;

[0025] Step 6: Close all valves, open valve e, valve f, valve g, turn on the vacuum pump to create a vacuum in the device, close valve f, valve g, open valve c, inject CO2 into the standard room, close valve c, and the pressure sensor c shows a stable reading of P S3 After that, open valve f. When the readings of pressure sensor c and pressure sensor d are the same and stable at P R4 When the carbon fixation of the filling body is calculated, the formula is as follows:

[0026]

[0027] Where P S3 is the initial CO2 pressure in the standard chamber, MPa; P R4 V is the CO2 pressure after stabilization in the reactor, MPa; R is the volume of the standard chamber, cm 3 ; V S is the pore volume of the reactor filling, cm 3 ; Z S3 , Z R4 are the compression factors of initial CO2 in the standard chamber and the compression factors of stabilized CO2 in the reactor, respectively, obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States; n b is the carbon fixation amount per unit mass of filling body, mmol / g; n b1 、n b2 are the initial amount of CO2 in the standard chamber, the amount of CO2 in the standard chamber and the reactor after the sealing begins, mmol; M is the mass of the filling body, g; R is the universal gas constant, 8.31 J / (mol・K); T is the temperature of the constant temperature water bath, K;

[0028] Step 7: When the CO2 injection time reaches the target number of days, close valve e and valve f, and according to the indication P of pressure sensor d, R5 Calculate the free storage volume of the filling body with the following formula:

[0029]

[0030] Where n f is the free storage capacity of the filling body, mmol / g; P R5 is the pressure in the reactor, MPa; V R is the volume of the standard chamber, cm 3 ; Z R5 is the compression factor of CO2 in the reactor, which is obtained by querying the carbon dioxide compression factor diagram at different temperatures and pressures; M is the mass of the filling body, g; R is the universal gas constant, 8.31 J / (mol・K); T is the temperature of the constant temperature water bath, K.

[0031] Preferably, the method further comprises a permeability test, and the specific steps are as follows:

[0032] Step 1: Place the filling body sample into a reactor, and connect the filling body to a negative carbon content test device for the whole process of carbon dioxide sealing;

[0033] Step 2: Close all valves, open valve d and valve e, inject He into the standard chamber, and then open valve f to perform air tightness test of the device;

[0034] Step 3: Close all valves, open valve e, valve f, valve g, and turn on the vacuum pump to establish the vacuum of the device;

[0035] Step 4: Set the temperature of the constant temperature water bath and apply axial pressure and confining pressure through the triaxial stress loading subsystem;

[0036] Step 5: Close all valves, open valve d and valve e, inject He into the standard chamber, close the valves, and wait until the pressure sensor c shows a stable reading of P. S1 After that, open valve f. When the readings of pressure sensor c and pressure sensor d are the same and stable at P R2 When the free space volume of the device is calculated, the calculation formula is as follows:

[0037]

[0038] Where V R is the volume of the standard chamber, cm 3 ; V S is the pore volume of the reactor filling, cm 3 ;P S1 is the initial He pressure in the standard chamber, MPa; P R2 is the He pressure in the reactor after stabilization, MPa; Z S1 , Z R2 They are the compression factor of the initial He in the standard chamber and the compression factor of the stabilized He in the reactor, respectively, which are obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States;

[0039] Step 6: Close all valves, open valve e, valve f, valve g, turn on the vacuum pump to create a vacuum in the device, close valve f, valve g, open valve c, inject CO2 into the standard chamber, close valve c, and wait until the pressure sensor c indicates a stable reading of P R6 After that, open valve f and valve j and start timing. Wait until the readings of pressure sensor c and pressure sensor d are the same and stable at P. R7 When the time is reached, stop timing, record the seepage time as T, and read the reading P of the pressure sensor e. R8, monitor the readings of the gas flow sensor and the electronic balance, and calculate the permeability of CO2 in the filling body. The calculation formula is:

[0040]

[0041] Where k is the CO2 permeability; μ is the dynamic viscosity of CO2, Pa·s; Q is the total seepage flow of CO2, m 3 ; L is the length of the filling body, m; A is the port cross-sectional area of ​​the filling body, m 2 ; T is the seepage time, s; P R6 , P R7 , P R8 They are the initial pressure at the reactor inlet, the final pressure at the reactor inlet, and the final pressure at the reactor outlet, in MPa.

[0042] As a preference, when the seepage rate does not exceed 0.001m 3 / min, the gas flow sensor is used to calculate the total seepage flow rate Q of CO2; when the seepage flow rate is greater than 0.001m 3 / min, the total seepage flow rate Q of CO2 is calculated by the water displacement method using an electronic balance.

[0043] Beneficial effects: Permeability and carbon fixation are two key parameters of the filling and sealing technology of carbon dioxide, which can characterize the sealing capacity of the filling body and the flow characteristics of CO2, and are important indicators for evaluating the effect of filling and sealing carbon dioxide. However, the carbon fixation test in the existing technology is mostly used for coal and rock samples, and only mineralization or adsorption carbon fixation is considered separately, without comprehensive consideration of the overall carbon fixation of the sample under various CO2 sealing effects such as mineralization, adsorption, dissolution, and free sealing, and the influence of CO2 injection time on the carbon fixation of the sample. Therefore, the present invention proposes a negative carbon content testing device and method for the whole process of carbon dioxide sealing by a filling body, which adopts a stress loading subsystem and a constant temperature control subsystem to simulate the actual filling and sealing conditions, and injects helium and carbon dioxide in turn through a high-pressure gas injection subsystem to measure the free space volume of the reactor and the negative carbon content and permeability of the filling body, and can accurately, real-timely and quickly monitor the negative carbon content and permeability of the whole process of carbon dioxide sealing by the filling body, thereby ensuring the reliability and accuracy of the test data. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 This is a schematic structural diagram of a device for testing the negative carbon content of a filling body during the entire process of carbon dioxide storage according to the present invention;

[0045] Figure 2 It is a schematic diagram of the structure of the reactor of the present invention;

[0046] Figure 3 It is a schematic diagram of a data acquisition unit of the present invention;

[0047] The numbers in the figure represent the following: 1. CO2 gas cylinder; 2. He gas cylinder; 3. Valve a; 4. Valve b; 5. Booster pump a; 6. Air compressor a; 7. Air compressor b; 8. Booster pump b; 9. Pressure sensor a; 10. Pressure sensor b; 11. Valve c; 12. Valve d; 13. High-pressure CO2 storage tank; 14. High-pressure He storage tank; 15. Standard room; 16. Valve e; 17. Pressure sensor c; 18. Valve f; 19. Pressure sensor d; 20. Reactor; 21. Pressure sensor e; 22. Valve g; 23. Valve h; 24. Buffer device; 25. Valve i; 26. Pressure sensor f; 27. Vacuum pump; 28. . Valve j; 29. ​​Gas flow sensor; 30. Condenser; 31. Saturated sodium bicarbonate solution storage tank; 32. Electronic balance; 33. Axial pressure pump; 34. Confining pressure pump; 35. Bracket; 36. Temperature sensor; 37. Constant temperature water bath; 38. Data analysis unit; 39. Data acquisition unit; 40. Data acquisition subsystem; 41. Reactor cylinder; 42. Piston; 43. Plug; 44. First clamping cap; 45. Second clamping cap; 46. First fixing ring; 47. Second fixing ring; 48. Filling body sample; 49. Rubber sleeve; 50. Confining pressure inlet; 51. Confining pressure cavity; 52. Axial pressure inlet; 53. Axial pressure cavity; 54. Air inlet; 55. Air outlet. DETAILED DESCRIPTION

[0048] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0049] Example

[0050] like Figure 1 As shown, a device for testing the negative carbon content of a filling body during the whole process of carbon dioxide sealing provided by an embodiment of the present invention includes: a filling body sealing carbonization subsystem, a high-pressure gas injection subsystem, a triaxial stress loading subsystem, a constant temperature control subsystem, a vacuum pumping subsystem, a data acquisition subsystem 40 and a seepage monitoring subsystem.

[0051] The main structure of the filling body sealing carbonization subsystem is the reactor 20, which is a horizontal tri-axial core clamp, in which the core is replaced by a filling body sample 48 (in this embodiment, the filling body sample 48 is a cylinder with a diameter of 50 mm and a height of 100 mm), including a confining pressure structure arranged around the filling body sample 48, an axial pressure structure arranged at one end of the filling body sample 48, and horizontal air inlet holes 54 and air outlet holes 55 arranged at both ends of the filling body sample 48. The confining pressure structure is provided with a confining pressure inlet 50, and the axial pressure structure is provided with an axial pressure inlet 52.

[0052] Further, such as Figure 2 As shown, the reactor 20 includes a reactor cylinder 41, a piston 42, a plug 43, a first clamping cap 44, a second clamping cap 45, a first fixing ring 46, a second fixing ring 47, and a rubber sleeve 49. The rubber sleeve 49 is axially arranged inside the reactor cylinder 41. The rubber sleeve 49 has a cavity that accommodates a filling body sample 48 to be tested and passes through the cavity axially. The first clamping cap 44 and the second clamping cap 45 are respectively embedded around the piston 42 and the plug 43 and are arranged at both ends of the reactor cylinder 41. The first fixing ring 46 and the second fixing ring 47 are respectively arranged at both ends of the rubber sleeve 49 and are respectively pressed against the inner ends of the first clamping cap 44 and the second clamping cap 45. The piston 42 passes through the first clamping cap 44 and is arranged at the second clamping cap 47. A fixed collar 46 has an internal cavity and can move left and right in the cavity. The plug 43 passes through the second clamping cap 45 and is arranged in the internal cavity of the second fixed collar 47, and the inner end of the plug 43 is pressed against the side end of the filling body sample 48. The axial center opening of the piston 42 and the plug 43 forms a horizontal air inlet 54 and an air outlet 55 for the air inlet and outlet of the filling body sample 48 at both ends; the outer wall of the rubber sleeve 49, the inner wall of the reactor cylinder 41 and the first fixed collar 46 and the second fixed collar 47 at both ends form a confining pressure chamber 51, and the confining pressure inlet 50 is arranged on the reactor cylinder 41; the cavity formed by the piston 42, the first clamping cap 44 and the first fixed collar 46 is an axial pressure chamber 53, and the axial pressure inlet 52 is arranged on the first clamping cap 44.

[0053] Furthermore, the reactor 20 further includes a bracket 35 , which is disposed at the bottom of the reactor 20 and is used to support the reactor 20 .

[0054] The high-pressure gas injection subsystem includes a standard chamber 15 (the volume is 100 mL in this embodiment), a CO2 boosting pipeline and a He boosting pipeline. The CO2 boosting pipeline includes a high-pressure CO2 storage tank 13, and the He boosting pipeline includes a high-pressure He storage tank 14. One end of the standard chamber 15 is connected to the high-pressure CO2 storage tank 13 and the high-pressure He storage tank 14 pipeline respectively, and the other end is connected to the air inlet 54 of the reactor 20. A valve c 11 and a pressure sensor a 9 are provided at the outlet of the high-pressure CO2 storage tank 13, a valve d 12 and a pressure sensor b 10 are provided at the outlet of the high-pressure He storage tank 14, a valve e 16 and a pressure sensor c 17 are provided at the outlet of the standard chamber 15, and a valve f 18 and a pressure sensor d 19 are provided at the air inlet 54 of the reactor 20.

[0055] Furthermore, the CO2 boosting pipeline also includes a CO2 gas cylinder 1, a boosting pump a5, and an air compressor a6. The CO2 gas cylinder 1, a valve a3, a boosting pump a5, a pressure sensor a9, a valve c11, and a high-pressure CO2 storage tank 13 are connected by pipelines in sequence. The pipeline between the pressure sensor a9 and the valve c11 is connected to the standard chamber 15. The air compressor a6 is connected to the boosting pump a5 to provide gas pressure. The He boosting pipeline also includes a He gas cylinder 2, a boosting pump b8, and an air compressor b7. The He gas cylinder 2, a valve b4, a boosting pump b8, a pressure sensor b10, a valve d12, and a high-pressure He storage tank 14 are connected by pipelines in sequence. The pipeline between the pressure sensor b10 and the valve d12 is connected to the standard chamber 15. The air compressor b7 and the boosting pump b8 are connected to provide gas pressure.

[0056] The triaxial stress loading subsystem includes an axial pressure pump 33 and a confining pressure pump 34 , and the axial pressure pump 33 and the confining pressure pump 34 are connected to the axial pressure inlet 52 and the confining pressure inlet 50 through pipelines respectively.

[0057] The constant temperature control subsystem includes a constant temperature water bath 37 and a temperature sensor 36 connected thereto. The constant temperature water bath 37 is arranged outside the reaction kettle 20 and the standard chamber 15 for adjusting the temperature.

[0058] The vacuum pumping subsystem includes a vacuum pump 27, which is connected to the gas outlet 55 of the reactor 20. A pressure sensor f 26 is provided at the inlet of the vacuum pump. A pressure sensor e 21 and a valve g 22 are provided at the gas outlet of the reactor 20 in sequence.

[0059] Furthermore, the vacuum pumping subsystem also includes a buffer device 24, which is arranged between the pipeline connected to the pressure sensor f26 and the valve g22, and a valve h23 is provided at the inlet of the buffer device 24, a valve i25 is provided at one outlet, and the other outlet is connected to the pressure sensor f26 pipeline.

[0060] The seepage monitoring subsystem includes a condenser 30, a saturated sodium bicarbonate solution storage tank 31, and an electronic balance 32 which are connected in sequence by pipelines. The air inlet end of the condenser 30 is connected to the air outlet 55 of the reactor 20 by pipeline. A valve j 28 and a gas flow sensor 29 are provided at the air inlet end of the condenser 30. The electronic balance 32 is used to weigh the mass of the solution discharged from the saturated sodium bicarbonate solution storage tank 31. The gas flow sensor 29 and the electronic balance 32 are electrically connected to the input end of the controller respectively.

[0061] The data acquisition subsystem 40 includes a data acquisition unit 39 and a data analysis unit 38. The data acquisition unit 39 includes a pressure sensor a 9, a pressure sensor b 10, a pressure sensor c 17, a pressure sensor d 19, a pressure sensor e 21, a pressure sensor f 26, a gas flow sensor 29, an electronic balance 32 and a temperature sensor 36. The data analysis unit 38 is a controller and a display. The input end of the controller is electrically connected to the pressure sensor a 9, the pressure sensor b 10, the pressure sensor c 17, the pressure sensor d 19, the pressure sensor e 21, the pressure sensor f 26, the gas flow sensor 29, the electronic balance 32 and the temperature sensor 36, respectively, and the output end is electrically connected to the display.

[0062] like Figure 3 As shown, the data types of the data acquisition unit 39 include gas pressure, loading stress, temperature and seepage rate. The gas pressure includes the pressure of the high-pressure CO2 storage tank, the pressure of the high-pressure He storage tank, the standard room pressure, the pressure at the inlet end of the reactor, the pressure at the outlet end of the reactor, and the vacuum pumping pressure. The loading stress specifically includes the axial pressure and the confining pressure. The temperature is the temperature of the constant temperature water bath. The seepage rate includes the gas flow at the outlet end of the reactor and the mass of the saturated sodium bicarbonate solution discharged.

[0063] A method for testing the negative carbon content of a filling body during the whole process of storing carbon dioxide based on the above filling body negative carbon content testing device for the whole process of storing carbon dioxide, the steps are as follows:

[0064] Step 1: Place the filling body sample 48 into a reactor, and connect the filling body to a negative carbon content test device for the whole process of carbon dioxide storage;

[0065] Step 2: Close all valves, open valve b4, valve d12, booster pump b8, and air compressor b7, inject He into the high-pressure He storage tank 14, and after reaching the preset gas pressure (16 MPa in this embodiment), close valve b4, booster pump b8, and air compressor b7, and open valve e16, inject He into the standard chamber 15, and then open valve f18 to perform air tightness test of the device. If the change in the reading of pressure sensor d19 during 2 hours is less than 0.002 MPa, it means that the equipment has good sealing performance;

[0066] Step 3: Close all valves, open valve e 16, valve f 18, valve g 22, valve h 23, turn on the vacuum pump 27 to establish the vacuum of the device, and when the reading of the pressure sensor f 26 becomes 0, turn off the vacuum pump;

[0067] Step 4: Set the temperature of the constant temperature water bath 37, apply axial pressure and confining pressure through the triaxial stress loading subsystem, the experimental temperature range is room temperature to 100° C., the axial pressure range is 0 to 20 MPa, and the confining pressure range is 0 to 20 MPa;

[0068] Step 5: Close all valves, open valve b4, valve d12, booster pump b8, and air compressor b7, and inject He into the high-pressure He storage tank 14. When the preset gas pressure (1-16 MPa) is reached, close valve b4, booster pump b8, and air compressor b7, and open valve e16 to inject He into the standard chamber 15. Wait until the pressure sensor c17 shows a stable reading of P S1 After that, close valve d12 and open valve f18. When the readings of pressure sensor c17 and pressure sensor d19 are the same and stable at P R2 When the free space volume of the device is calculated, the calculation formula is as follows:

[0069]

[0070] Where V R is the volume of the standard chamber, cm 3 ; V S is the pore volume of the reactor filling, cm 3 ;P S1 is the initial He pressure in the standard chamber, MPa; P R2 is the He pressure in the reactor after stabilization, MPa; Z S1 , Z R2 are the compression factor of the initial He in the standard chamber and the compression factor of the stabilized He in the reactor, respectively, which are obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States (see Table 1 below);

[0071] Table 1 Helium compression factor at 0-16 MPa, 20-100°C

[0072]

[0073] Step 6. Close all valves, open valve e16, valve f18, valve g22, valve h23, open vacuum pump 27 to establish vacuum in the device. When the pressure sensor f26 indicates 0, turn off vacuum pump 27, close valve f18, valve g22, valve h23, open valve a3, valve c11, booster pump a5, air compressor a6 to inject CO2 into high-pressure CO2 storage tank 13. When the preset gas pressure (1~16MPa) is reached, close valve a3, booster pump a5, air compressor a6, open valve e16, inject CO2 into standard chamber 15, and the pressure sensor c17 indicates a stable reading of P.S3 After that, close valve c11 and open valve f18. When the readings of pressure sensor c17 and pressure sensor d19 are the same and stable at P R4 When the carbon fixation of the filling body is calculated, the formula is as follows:

[0074]

[0075] Where P S3 is the initial CO2 pressure in the standard chamber, MPa; P R4 V is the CO2 pressure after stabilization in the reactor, MPa; R is the volume of the standard chamber, cm 3 ; V S is the pore volume of the reactor filling, cm 3 ; Z S3 , Z R4 are the compression factors of the initial CO2 in the standard chamber and the compression factors of the stabilized CO2 in the reactor, respectively, obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States (see Table 2 below); n b is the carbon fixation amount per unit mass of filling body, mmol / g; n b1 、n b2 are the initial amount of CO2 in the standard chamber, the amount of CO2 in the standard chamber and the reactor after the sealing begins, mmol; M is the mass of the filling body, g; R is the universal gas constant, 8.31 J / (mol・K); T is the temperature of the constant temperature water bath, K;

[0076] Table 2 Compression factor of carbon dioxide at 0-16 MPa, 20-100°C

[0077]

[0078] Step 7: When the CO2 injection time reaches the target number of days (1 to 7 days), close valve e 16 and valve f 18, and according to the reading P of pressure sensor d 19 R5 Calculate the free storage volume of the filling body with the following formula:

[0079]

[0080] Where n f is the free storage capacity of the filling body, mmol / g; P R5 is the pressure in the reactor, MPa; V R is the volume of the standard chamber, cm 3 ; Z R5is the compression factor of CO2 in the reactor, obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States (see Table 2 above); M is the mass of the filling body, g; R is the universal gas constant, 8.31 J / (mol・K); T is the temperature of the constant temperature water bath, K.

[0081] Furthermore, as one of the preferred embodiments of the present invention, the method further includes a permeability test, and the specific steps are as follows:

[0082] Step 1: Place the filling body sample 48 into a reactor, and connect the filling body to a negative carbon content test device for the whole process of carbon dioxide storage;

[0083] Step 2: Close all valves, open valve b4, valve d12, booster pump b8, and air compressor b7, inject He into the high-pressure He storage tank 14, and after reaching the preset gas pressure (16 MPa in this embodiment), close valve b4, booster pump b8, and air compressor b7, and open valve e16, inject He into the standard chamber 15, and then open valve f18 to perform air tightness test of the device. If the change in the reading of pressure sensor d19 during 2 hours is less than 0.002 MPa, it means that the equipment has good sealing performance;

[0084] Step 3: Close all valves, open valve e 16, valve f 18, valve g 22, valve h 23, turn on the vacuum pump 27 to establish the vacuum of the device, and when the reading of the pressure sensor f 26 becomes 0, turn off the vacuum pump;

[0085] Step 4: Set the temperature of the constant temperature water bath 37, apply axial pressure and confining pressure through the triaxial stress loading subsystem, the experimental temperature range is room temperature to 100° C., the axial pressure range is 0 to 20 MPa, and the confining pressure range is 0 to 20 MPa;

[0086] Step 5: Close all valves, open valve b4, valve d12, booster pump b8, and air compressor b7, and inject He into the high-pressure He storage tank 14. When the preset gas pressure (1-16 MPa) is reached, close valve b4, booster pump b8, and air compressor b7, and open valve e16 to inject He into the standard chamber 15. Wait until the pressure sensor c17 shows a stable reading of P S1 After that, close valve d12 and open valve f18. When the readings of pressure sensor c17 and pressure sensor d19 are the same and stable at P R2 When the free space volume of the device is calculated, the calculation formula is as follows:

[0087]

[0088] Where VR is the volume of the standard chamber, cm 3 ; V S is the pore volume of the reactor filling, cm 3 ;P S1 is the initial He pressure in the standard chamber, MPa; P R2 is the He pressure in the reactor after stabilization, MPa; Z S1 , Z R2 are the compression factor of the initial He in the standard chamber and the compression factor of the stabilized He in the reactor, respectively, which are obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States (see Table 1);

[0089] Step 6. Close all valves, open valve e16, valve f18, valve g22, valve h23, open vacuum pump 27 to establish vacuum in the device, and when the indication of pressure sensor f26 becomes 0, turn off vacuum pump 27; close valve f18, valve g22, valve h23, open valve a3, valve c11, booster pump a5, air compressor a6 to inject CO2 into high-pressure CO2 storage tank 13, and when the preset gas pressure (1~16MPa) is reached, close valve a3, booster pump a5, air compressor a6 and open valve e16, inject CO2 into standard chamber 15, and wait until the indication of pressure sensor c17 stabilizes to P R6 After that, close valve c 11, open valve f 18 and valve j 28 and start timing, wait until the readings of pressure sensor c 17 and pressure sensor d 19 are the same and stable at P R7 When the time is reached, stop timing, record the seepage time as T, and read the reading P of the pressure sensor e21. R8 , monitor the readings of the gas flow sensor 29 and the electronic balance 32, and calculate the permeability of CO2 in the filling body. The calculation formula is:

[0090]

[0091] Where k is the CO2 permeability; μ is the dynamic viscosity of CO2, Pa·s, which can be obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States (see Table 3); Q is the total seepage flow rate of CO2, m 3 ; L is the length of the filling body, m; A is the port cross-sectional area of ​​the filling body, m 2 ; T is the seepage time, s; P R6 , P R7 , P R8 They are the initial pressure at the reactor inlet, the final pressure at the reactor inlet, and the final pressure at the reactor outlet, in MPa.

[0092] Table 3 Dynamic viscosity of carbon dioxide at 0-16 MPa, 20-100°C

[0093]

[0094] Furthermore, as one of the preferred embodiments of the present invention, when the seepage volume is less than or equal to 0.001m 3 / min, the gas flow sensor 29 is used to calculate the total seepage flow Q of CO2; when the seepage flow is greater than 0.001m 3 / min, the total seepage flow rate Q of CO2 is calculated by the electronic balance 32 using the water displacement method.

[0095] Finally, it should be noted that the above implementation modes are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned implementation modes, a person of ordinary skill in the art should understand that the technical solutions described in the aforementioned implementation modes can still be modified, or some or all of the technical features therein can be replaced by equivalents. However, these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the implementation modes of the present invention.

Claims

1. A device for testing the negative carbon content of a filling body during the whole process of carbon dioxide storage, characterized in that: The testing device comprises: a filling body sealing and carbonization subsystem, a high-pressure gas injection subsystem, a triaxial stress loading subsystem, a constant temperature control subsystem, a vacuum pumping subsystem and a data acquisition subsystem (40). The main structure of the filling body sealing carbonization subsystem is a reactor (20), which is a horizontal triaxial core holder for replacing the rock sample with the filling body sample (48). The reactor (20) comprises a confining pressure structure arranged around the filling body sample (48), an axial pressure structure arranged at one end of the filling body sample (48), and horizontal air inlet holes (54) and air outlet holes (55) arranged at both ends of the filling body sample (48). The confining pressure structure is provided with a confining pressure inlet (50), and the axial pressure structure is provided with an axial pressure inlet (52); The high-pressure gas injection subsystem comprises a standard chamber (15), a CO2 boosting pipeline and a He boosting pipeline, the CO2 boosting pipeline comprises a high-pressure CO2 storage tank (13), the He boosting pipeline comprises a high-pressure He storage tank (14), one end of the standard chamber (15) is respectively connected to the pipelines of the high-pressure CO2 storage tank (13) and the high-pressure He storage tank (14), and the other end is connected to the air inlet (54) of the reactor (20), the high-pressure CO2 storage tank (13) is provided with a valve c (11) and a pressure sensor a (9) at the outlet, the high-pressure He storage tank (14) is provided with a valve d (12) and a pressure sensor b (10) at the outlet, the standard chamber (15) is provided with a valve e (16) and a pressure sensor c (17) at the outlet, and the air inlet of the reactor (20) is provided with a valve f (18) and a pressure sensor d (19); The triaxial stress loading subsystem comprises an axial pressure pump (33) and a confining pressure pump (34), wherein the axial pressure pump (33) and the confining pressure pump (34) are respectively connected to the axial pressure inlet (52) and the confining pressure inlet (50) pipelines; The constant temperature control subsystem comprises a constant temperature water bath (37) and a temperature sensor (36) connected thereto, wherein the constant temperature water bath (37) is arranged outside the reaction kettle (20) and the standard chamber (15) and is used to adjust the temperature; The vacuum pump subsystem comprises a vacuum pump (27), the vacuum pump (27) is connected to the gas outlet (55) of the reaction kettle (20), a pressure sensor f (26) is provided at the inlet of the vacuum pump, and a pressure sensor e (21) and a valve g (22) are provided at the gas outlet (55) of the reaction kettle (20) in sequence; The data acquisition subsystem (40) includes a data acquisition unit (39) and a data analysis unit (38). The data acquisition unit (39) includes a pressure sensor a (9), a pressure sensor b (10), a pressure sensor c (17), a pressure sensor d (19), a pressure sensor e (21), a pressure sensor f (26), and a temperature sensor (36). The data analysis unit (38) is a controller and a display. An input end of the controller is electrically connected to the pressure sensor a (9), the pressure sensor b (10), the pressure sensor c (17), the pressure sensor d (19), the pressure sensor e (21), the pressure sensor f (26), and the temperature sensor (36), respectively, and an output end is electrically connected to the display.

2. The device for testing the negative carbon content of the whole process of carbon dioxide storage by a filling body according to claim 1 is characterized in that: The filling body carbon dioxide sealing whole process negative carbon content testing device also includes a seepage monitoring subsystem, the seepage monitoring subsystem includes a condenser (30), a saturated sodium bicarbonate solution storage tank (31), and an electronic balance (32) which are connected in sequence by pipelines, the air inlet end of the condenser (30) is connected to the air outlet (55) of the reactor (20) by a pipeline, a valve j (28) and a gas flow sensor (29) are provided at the air inlet end of the condenser (30), the electronic balance (32) is used to weigh the mass of the solution discharged from the saturated sodium bicarbonate solution storage tank (31), and the gas flow sensor (29) and the electronic balance (32) are respectively electrically connected to the input end of the controller.

3. The device for testing the negative carbon content of the whole process of carbon dioxide storage by a filling body according to claim 1 is characterized in that: The CO2 boosting pipeline further comprises a CO2 gas cylinder (1), a boosting pump a (5), and an air compressor a (6); the CO2 gas cylinder (1), a valve a (3), a boosting pump a (5), a pressure sensor a (9), a valve c (11), and a high-pressure CO2 storage tank (13) are connected in sequence by pipelines; a pipeline between the pressure sensor a (9) and the valve c (11) is connected to a standard chamber (15); and the air compressor a (6) is connected to the boosting pump a (5) for providing gas pressure; the He boosting pipeline further comprises a He gas cylinder (2), a boosting pump b (8), and an air compressor b (7); the He gas cylinder (2), a valve b (4), a boosting pump b (8), a pressure sensor b (10), a valve d (12), and a high-pressure He storage tank (14) are connected in sequence by pipelines; a pipeline between the pressure sensor b (10) and the valve d (12) is connected to the standard chamber (15); and the air compressor b (7) and the boosting pump b (8) are connected for providing gas pressure.

4. The device for testing the negative carbon content of the whole process of carbon dioxide storage by a filling body according to claim 1, characterized in that: The reactor (20) comprises a reactor cylinder (41), a piston (42), a plug (43), a first clamping cap (44), a second clamping cap (45), a first fixing ring (46), a second fixing ring (47), and a rubber sleeve (49). The rubber sleeve (49) is axially arranged inside the reactor cylinder (41). The rubber sleeve (49) has a cavity that accommodates a filling body sample (48) to be tested and is axially penetrated. The first clamping cap (44) and the second clamping cap (45) are respectively embedded around the piston (42) and the plug (43) and are arranged at two ends of the reactor cylinder (41). The first fixing ring (46) and the second fixing ring (47) are respectively arranged at two ends of the rubber sleeve (49) and are respectively pressed against the inner ends of the first clamping cap (44) and the second clamping cap (45). The piston (42) passes through the first clamping cap (44) and is arranged at the first The fixing ring (46) has an internal cavity and can move left and right in the cavity. The plug (43) passes through the second clamping cap (45) and is arranged in the internal cavity of the second fixing ring (47). The inner side end of the plug (43) abuts against the side end of the filling body sample (48). The axial center openings of the piston (42) and the plug (43) form horizontal air inlet holes (54) and air outlet holes (55) for air inlet and outlet at both ends of the filling body sample (48). The outer wall of the rubber sleeve (49), the inner wall of the reactor cylinder (41) and the first fixing ring (46) and the second fixing ring (47) at both ends form a confining pressure cavity (51), and the confining pressure inlet (50) is arranged on the reactor cylinder (41). The cavity formed by the piston (42), the first clamping cap (44) and the first fixing ring (46) is an axial pressure cavity (53), and the axial pressure inlet (52) is arranged on the first clamping cap (44).

5. The device for testing the negative carbon content of the whole process of carbon dioxide storage by a filling body according to claim 1 is characterized in that: The reaction kettle (20) further comprises a support (35), wherein the support (35) is arranged at the bottom of the reaction kettle (20) and is used to support the reaction kettle (20).

6. The device for testing the negative carbon content of the whole process of carbon dioxide storage by a filling body according to claim 1, characterized in that: The vacuum pumping subsystem further comprises a buffer device (24), which is arranged between a pipeline connected to the pressure sensor f (26) and the valve g (22), and a valve h (23) is arranged at an inlet of the buffer device (24), a valve i (25) is arranged at one outlet, and the other outlet is connected to the pipeline of the pressure sensor f (26).

7. A method for testing the negative carbon content of a filling body during the whole process of storing carbon dioxide based on the device for testing the negative carbon content of a filling body during the whole process of storing carbon dioxide according to claim 1, characterized in that: Here are the steps: Step 1: placing a filling body sample (48) into a reaction kettle, and connecting the filling body to a negative carbon content testing device for the entire process of carbon dioxide storage; Step 2: Close all valves, open valve d (12) and valve e (16), inject He into the standard chamber (15), and then open valve f (18) to perform air tightness test of the device; Step 3: Close all valves, open valve e (16), valve f (18), valve g (22), and turn on the vacuum pump (27) to establish a vacuum in the device; Step 4, setting the temperature of the constant temperature water bath (37), and applying axial pressure and confining pressure through the triaxial stress loading subsystem; Step 5: Close all valves, open valve d (12) and valve e (16), inject He into the standard chamber (15), close valve d (12), and wait until the pressure sensor c (17) indicates a stable reading of P S1 After that, open valve f (18). When the readings of pressure sensor c (17) and pressure sensor d (19) are the same and stable at P R2 When the free space volume of the device is calculated, the calculation formula is as follows: ， Where V R is the volume of the standard chamber, cm 3 ; V S is the pore volume of the reactor filling, cm 3 ;P S1 is the initial He pressure in the standard chamber, MPa; P R2 is the He pressure after stabilization in the reactor, MPa; Z S1 , Z R2 They are the compression factor of the initial He in the standard chamber and the compression factor of the stabilized He in the reactor, respectively, which are obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States; Step 6: Close all valves, open valve e (16), valve f (18), valve g (22), open the vacuum pump (27) to create a vacuum in the device, close valve f (18) and valve g (22), open valve c (11), inject CO2 into the standard chamber (15), close valve c (11), and the pressure sensor c (17) indicates a stable reading of P S3 After that, open valve f (18). When the readings of pressure sensor c (17) and pressure sensor d (19) are the same and stable at P R4 When the negative carbon content of the filling body is calculated, the formula is as follows: ， Where P S3 is the initial CO2 pressure in the standard chamber, MPa; P R4 V is the CO2 pressure after stabilization in the reactor, MPa; R is the volume of the standard chamber, cm 3 ; V S is the pore volume of the reactor filling, cm 3 ; Z S3 , Z R4 are the compression factors of initial CO2 in the standard chamber and the compression factors of stabilized CO2 in the reactor, respectively, obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States; n b is the carbon fixation amount per unit mass of filling body, mmol / g; n b1 、n b2 are the initial amount of CO2 in the standard chamber, the amount of CO2 in the standard chamber and the reactor after the sealing begins, mmol; M is the mass of the filling body, g; R is the universal gas constant, 8.31 J / (mol・K); T is the temperature of the constant temperature water bath, K; Step 7: When the CO2 injection time reaches the target number of days, close valve e (16) and valve f (18), and according to the indication P of pressure sensor d (19), R5 Calculate the free storage capacity of CO2 in the filling body using the following formula: ， Where n f is the free storage capacity of CO2 in the filling body, mmol / g; P R5 is the pressure in the reactor, MPa; V R is the volume of the standard chamber, cm 3 ; Z R5 is the compression factor of CO2 in the reactor, which is obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States; M is the mass of the filling body, g; R is the universal gas constant, 8.31 J / (mol・K); T is the temperature of the constant temperature water bath, K.

8. A method for testing the negative carbon content of a filling body during the whole process of storing carbon dioxide based on the device for testing the negative carbon content of a filling body during the whole process of storing carbon dioxide according to claim 2, characterized in that: The method includes a permeability test of the filling body, and the specific steps are as follows: Step 1, placing a filling body sample (48) into a reaction kettle, and connecting the filling body to a negative carbon content testing device for the entire process of carbon dioxide storage; Step 2: Close all valves, open valve d (12) and valve e (16), inject He into the standard chamber (15), and then open valve f (18) to perform air tightness test of the device; Step 3: Close all valves, open valve e (16), valve f (18), valve g (22), and turn on the vacuum pump (27) to establish a vacuum in the device; Step 4, setting the temperature of the constant temperature water bath (37), and applying axial pressure and confining pressure through the triaxial stress loading subsystem; Step 5: Close all valves, open valve d (12) and valve e (16), inject He into the standard chamber (15), close valve d (12), and wait until the pressure sensor c (17) indicates a stable reading of P S1 After that, open valve f (18). When the readings of pressure sensor c (17) and pressure sensor d (19) are the same and stable at P R2 When the free space volume of the device is calculated, the calculation formula is as follows: ， Where V R is the volume of the standard chamber, cm 3 ; V S is the pore volume of the reactor filling, cm 3 ;P S1 is the initial He pressure in the standard chamber, MPa; P R2 is the He pressure after stabilization in the reactor, MPa; Z S1 , Z R2 They are the compression factor of the initial He in the standard chamber and the compression factor of the stabilized He in the reactor, respectively, which are obtained by querying the REFPROP physical property database software developed by the National Institute of Standards and Technology of the United States; Step 6: Close all valves, open valve e (16), valve f (18), valve g (22), open the vacuum pump (27) to create a vacuum in the device, close valve f (18) and valve g (22), open valve c (11), inject CO2 into the standard chamber (15), close valve c (11), and wait until the pressure sensor c (17) indicates a stable reading of P R6 After that, open valve f (18) and valve j (28) and start timing. Wait until the readings of pressure sensor c (17) and pressure sensor d (19) are the same and stable at P. R7 When the time is reached, stop timing, record the seepage time as T, and read the reading P of the pressure sensor e (21). R8 , monitor the readings of the gas flow sensor (29) and the electronic balance (32), and calculate the permeability of CO2 in the filling body. The calculation formula is: ， Where k is the CO2 permeability; μ is the dynamic viscosity of CO2, Pa·s; Q is the total seepage flow of CO2, m 3 ; L is the length of the filling body, m; A is the port cross-sectional area of ​​the filling body, m 2 ; T is the seepage time, s; P R6 , P R7 , P R8 They are the initial pressure at the reactor inlet, the final pressure at the reactor inlet, and the final pressure at the reactor outlet, in MPa.

9. The method for testing the negative carbon content of a filling body during the whole process of carbon dioxide storage according to claim 8, characterized in that: When the seepage rate does not exceed 0.001m 3 / min, the gas flow sensor (29) is used to calculate the total seepage flow rate Q of CO2; when the seepage flow rate is greater than 0.001m 3 / min, the total seepage flow rate Q of CO2 was calculated by the water displacement method using an electronic balance (32).

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