A high-temperature, high-pressure mixed CO2 mineralization reaction apparatus and method containing impurities

Abstract

The application discloses a high-temperature and high-pressure mixed CO2 mineralization reaction device and method containing impurities, which comprises a gas supply module, a gas mixer, a mixed gas analysis module, a mineralization reactor, a vacuum pumping module and a tail gas treatment module, wherein the gas supply module is used for providing CO2 gas and impurity gas, the gas mixer is used for mixing the CO2 gas and the impurity gas, the mixed gas analysis module is used for judging whether the CO2 gas and the impurity gas are uniformly mixed, the mineralization reactor is used for simulating mineralization reaction of a rock sample to be mineralized under the condition of the mixed CO2 gas containing impurities and environmental simulation liquid, the vacuum pumping module is used for pumping the mineralization reactor, and the tail gas treatment module is used for treating tail gas generated in the mineralization reaction. The application develops a device capable of simulating a formation water vapor evaporation environment, so that natural conditions can be more realistically reproduced in experiments, which will help better understand the performance of the mineralization reaction under actual geological conditions and improve the practicability of research.

Description

Technical Field

[0001] This invention belongs to the field of CO2 mineralization technology, specifically relating to a high-temperature, high-pressure mixed CO2 mineralization reaction device and method containing impurities. Background Technology

[0002] Gas mineralization (CMS) is an emerging carbon dioxide capture and storage (CCS) technology that permanently stores CO2 by reacting it with mineral-containing materials to form stable solid carbonates. In recent years, with the increasing severity of climate change and the growing global demand for CO2 emission control and reduction, CCS technology has received widespread attention and research. Currently, CO2 saline aquifer sequestration is an important technology for addressing climate change and reducing greenhouse gas emissions. Its basic principle is to inject captured CO2 into deep saline aquifers (i.e., groundwater containing saline water) for long-term storage and secure isolation. The reactivity of CO2-saline water-rock is crucial for the monitoring and validation of CO2 saline aquifer sequestration projects, requiring rapid analysis through laboratory studies, particularly experiments on the reaction of impurity CO2 with saline water and rocks.

[0003] In laboratory experiments, simulating the mineralization reaction of impurity-laden CO2 mixtures with rocks and saline water under simulated formation temperature and pressure conditions is a crucial step. However, actual formation conditions typically involve high-temperature and high-pressure environments, and the mineral composition and saline water chemical composition within different formations are complex and variable. Therefore, accurately simulating these conditions in laboratory or industrial environments, achieving efficient mineralization reactions of impurity-laden CO2 gases, and monitoring the water content of the reacting gases have become key areas of technological research and development.

[0004] To overcome these challenges, researchers need to develop more advanced experimental equipment and techniques to simulate formation conditions under high temperature and pressure. Simultaneously, the design of the reaction vessel is crucial. Complex designs and difficult operation, especially when handling gases containing impurities, make it difficult to precisely control the rate and quality of gas mixing and injection. This leads to uneven mixing of gas and solid / liquid, low reaction efficiency, and poor experimental reproducibility. Furthermore, current technologies cannot effectively simulate the environment of formation water vapor evaporation, limiting the monitoring of water content in the gas during the mineralization reaction. Therefore, improving the design and control precision of the reaction system is key to achieving efficient gas mineralization. Summary of the Invention

[0005] To address the problems existing in the prior art, this invention provides a high-temperature, high-pressure mixed CO2 mineralization reaction apparatus and method containing impurities. This invention develops an apparatus capable of simulating the evaporation environment of formation water vapor, so as to more realistically reproduce natural conditions in experiments. This will help to better understand the performance of mineralization reactions under actual geological conditions and improve the practicality of the research.

[0006] The technical solution adopted to achieve the above-mentioned objectives of this invention is as follows:

[0007] A high-temperature, high-pressure CO2 mineralization reaction device containing impurities includes a gas supply module, a gas mixer, a mixed gas analysis module, a mineralization reactor, a vacuum module, and a tail gas treatment module.

[0008] The gas supply module includes a CO2 gas supply unit and one or more impurity gas supply units;

[0009] The gas mixer includes a gas mixer housing, a primary spiral mixing tube, and a mixed gas output tube. The primary spiral mixing tube is spiral-shaped and has multiple outlet holes evenly distributed along its length. The primary spiral mixing tube is fixed inside the gas mixer housing. The gas mixer housing has an inlet. The CO2 gas supply unit and each impurity gas supply unit are respectively connected to the inlet. One end of the primary spiral mixing tube is connected to the outlet of the inlet, and the other end of the primary spiral mixing tube is closed. The gas mixer housing has a first outlet. One end of the mixed gas output tube is connected to the first outlet. A booster pump is installed on the mixed gas output tube. The mixed gas analysis module is connected to the mixed gas output tube.

[0010] The mineralization reactor includes a reactor shell, inside which is a support for placing rock samples. At the bottom of the reactor shell is an inverted conical gas inlet, and at the same bottom is an annular storage trough located around the gas inlet. A water inlet / outlet pipe is connected to the storage trough, with one end connected to the storage trough and a first control valve attached to it. A pressure gauge and a temperature sensor are connected to the reactor shell. The other end of a mixed gas output pipe is connected to the gas inlet. A vacuum module and a tail gas treatment module are connected to the reactor shell.

[0011] The CO2 gas supply unit includes a CO2 cylinder and a first supply pipe. The first supply pipe is equipped with a first gas flow meter, and one end of the first supply pipe is connected to the outlet of the CO2 cylinder. There are two impurity gas supply units: an SO2 gas supply unit and a NO2 gas supply unit. The SO2 gas supply unit includes an SO2 cylinder and a second supply pipe. The second supply pipe is equipped with a second gas flow meter, and one end of the second supply pipe is connected to the outlet of the SO2 cylinder. The NO2 gas supply unit includes an NO2 cylinder and a third supply pipe. The third supply pipe is equipped with a third gas flow meter, and one end of the third supply pipe is connected to the outlet of the NO2 cylinder. The other ends of the first, second, and third supply pipes are connected to the inlet via a four-way valve.

[0012] The gas mixer further includes a secondary mixing chamber and a stirring assembly. The secondary mixing chamber is located within the spiral space of the primary spiral mixing tube. The secondary mixing chamber has multiple evenly distributed air inlets. The stirring assembly can stir the mixed gas in the secondary mixing chamber. The secondary mixing chamber has a second air outlet, and an air outlet pipe is connected to the second air outlet. One end of the air outlet pipe is connected to the second air outlet, and the air outlet pipe passes through the first air outlet. A second control valve is provided on the air outlet pipe, and one end of the mixed gas output pipe is connected to the other end of the air outlet pipe.

[0013] The stirring assembly includes a stirring motor, a stirring shaft, and multiple stirring blades. The stirring motor is located outside the gas mixer housing and is fixed to one end face of the gas mixer housing. One end of the stirring shaft is connected to the output shaft of the stirring motor. The stirring shaft is parallel to the spiral extension direction of the primary spiral mixing pipe and passes through opposite sides of the secondary mixing chamber. The stirring shaft is rotatably connected to the secondary mixing chamber. The multiple stirring blades are located inside the secondary mixing chamber and are evenly distributed along the length of the stirring shaft.

[0014] The mineralization reactor is equipped with a microporous filter plate, which seals the top of the container and the gas injection port. The microporous filter plate is fixed to the bottom of the reactor shell. The top of the gas injection port is provided with an annular sealing groove, and a sealing ring is provided in the sealing groove.

[0015] The gas injection port tip is connected to a gas injection tube, one side of which is fixed to the bottom of the reactor shell, and one end of which is connected to the gas injection port.

[0016] The vacuum module includes a vacuum tube and a vacuum pump. One end of the vacuum tube is connected to the reactor shell, and the other end of the vacuum tube is connected to the vacuum pump. A third control valve is provided on the vacuum tube.

[0017] It also includes an exhaust gas treatment module, which includes an exhaust pipe and an exhaust gas treatment device. One end of the exhaust pipe is connected to the reactor shell, and the other end of the exhaust pipe is connected to the exhaust gas treatment device.

[0018] It also includes a gas sampling module, which includes a gas sampling container, a gas sampling tube, a temperature and humidity sensor, and a gas chromatograph. The two ends of the gas sampling tube are connected to the reactor shell and the gas sampling container. A fourth control valve is provided on the gas sampling tube. The temperature and humidity sensor is installed on the gas sampling container. The gas chromatograph is connected to the gas sampling container.

[0019] It also includes a liquid sampling module, which includes a liquid sampling container and a liquid sampling tube. One end of the liquid sampling tube is detachably connected to the other end of the inlet / outlet pipe, and the other end of the liquid sampling tube is connected to the liquid sampling container.

[0020] The mixed gas analysis module includes an analysis gas tube and a gas analyzer. The analysis gas tube is equipped with a fifth control valve. The two ends of the analysis gas tube are connected to the mixed gas output tube and the gas analyzer, respectively. The connection between the analysis gas tube and the mixed gas output tube is located between the booster pump and the gas outlet tube.

[0021] A mineralization method based on the aforementioned high-temperature, high-pressure impurity-containing mixed CO2 mineralization reaction device includes the following steps:

[0022] S1. Place the rock sample to be mineralized into the reactor shell;

[0023] S2. Turn on the CO2 gas supply unit and each impurity gas supply unit. CO2 gas and one or more impurity gases enter the gas mixer housing for mixing. When the amount of CO2 gas and each impurity gas entering the gas mixer housing reaches the set amount, turn off the CO2 gas supply unit and each impurity gas supply unit. After the CO2 gas and one or more impurity gases are fully mixed and homogeneous in the gas mixer housing, a mixed gas is obtained.

[0024] S3. Turn on the mixed gas analysis module and the second control valve to test the composition of the mixed gas. If the composition ratio of the mixed gas meets the requirements, stop mixing. If the composition ratio of the mixed gas does not meet the requirements, continue mixing until the mixed gas meets the test requirements. Then turn off the mixed gas analysis module and the second control valve.

[0025] S4. Turn on the vacuum module to evacuate the reactor shell. Once the reactor shell is under vacuum, turn off the vacuum module.

[0026] S5. Open the first control valve and inject the environmental simulation liquid into the holding tank through the injection and drainage pipe, then close the first control valve.

[0027] S6. Heat the reactor shell until it reaches the set temperature, then keep it warm.

[0028] S7. Open the second control valve and the booster pump to inject mixed gas into the reactor shell. At the same time, use the mixed gas to pressurize the reactor shell. When the pressure inside the reactor shell reaches the pressure required for the mineralization reaction, close the second control valve and the booster pump.

[0029] S8. The mineralization reaction begins inside the reactor shell. After the mineralization reaction is completed, heating of the reactor shell is stopped, and the tail gas treatment module is turned on to treat the tail gas generated by the mineralization reaction.

[0030] S9. Once the pressure inside the reactor shell has dropped to atmospheric pressure, remove the rock sample.

[0031] Furthermore, during the mineralization reaction, if it is necessary to perform component analysis and monitor temperature and humidity of the mixed gas during the mineralization reaction, the fourth control valve can be opened, and the mixed gas in the reactor shell can enter the gas sampling container for analysis by a gas chromatograph and temperature and humidity monitoring by a temperature and humidity sensor; if it is necessary to perform liquid analysis on the environmental simulation liquid in the placement tank during the mineralization reaction, the first control valve can be opened, and the environmental simulation liquid in the placement tank can flow into the liquid sampling container.

[0032] Compared with the prior art, the advantages and beneficial effects of the present invention are as follows:

[0033] 1. The gas mixer of the present invention has a good mixing effect, making CO2 and impurity gases more uniformly mixed. Moreover, the gas mixer of the present invention can mix different types of gases to adapt to various reaction requirements. This adaptability enables the system to play a role in different industrial applications and meet diverse laboratory / market needs.

[0034] 2. This invention can simulate the mineralization reaction of pure CO2, as well as the mineralization reaction of CO2 tail gas emitted in actual industrial processes (CO2 tail gas may contain various impurities, such as sulfides, nitrogen oxides, hydrocarbons, etc.), thus expanding the scope of application and showing great research and development prospects.

[0035] 3. This invention includes the design of water vapor evaporation control. By controlling the content of liquid components, reaction temperature and pressure in the environmental simulation, it simulates the actual formation liquid water-water vapor coexistence environment and realizes water vapor evaporation control, thereby realistically reproducing the natural conditions of CO2 mineralization reaction, improving the accuracy and reliability of the simulated CO2 mineralization reaction experimental results, and thus enhancing the value of CO2 mineralization reaction research.

[0036] 4. This invention can not only realize gas mixing and mineralization reaction, but also sample and analyze the mixed gas and environmental simulated liquid during the mineralization reaction process. This multi-functionality allows the device of this invention to flexibly meet different needs during the experiment, thus improving the wide applicability of this invention. Attached Figure Description

[0037] Figure 1 This is a schematic diagram of a high-temperature, high-pressure CO2 mineralization reaction device containing impurities.

[0038] Figure 2 This is a schematic diagram of a gas mixer.

[0039] Figure 3 This is a schematic diagram of the mineralization reactor.

[0040] Among them, 1-Gas supply module:

[0041] 11-CO2 gas supply unit: 11a-CO2 gas cylinder, 11b-first gas supply pipe, 11c-first gas flow meter;

[0042] 2-Gas Mixer:

[0043] 21-Gas mixer housing; 21a-Air inlet, 21b-First air outlet; 22-First stage spiral mixing pipe; 23-Second stage mixing chamber: 23a-Second air outlet; 24-Mixed gas output pipe; 25-First support; 26-Air outlet pipe; 27-Second check valve; 28-Agitator motor; 29-Agitator shaft; 210-Agitator blades; 211-Booster pump;

[0044] 3-Mineralization reactor:

[0045] 31-Reactor shell; 31a-Top cover; 31a1-Functional interface; 31b-Reaction cylinder; 31b1-Gas injection port; 32-Second support; 33-Insulation layer; 34-Pressure gauge; 35-Temperature sensor; 36-Gas injection pipe; 37-Container tank; 38-Injection and drainage pipe; 39-First one-way valve; 310-Microporous filter plate; 311-Annular pressure plate; 312-Stud; 313-Sealing ring; 314-First tee; 315-Rock sample support;

[0046] 4-Mixed Gas Analysis Module:

[0047] 41-Analytical gas tube; 42-Second three-way valve; 43-Gas analyzer; 44-Fifth check valve;

[0048] 5-Vacuum Pumping Module:

[0049] 51-Vacuum tube; 52-Vacuum pump; 53-Third check valve;

[0050] 6-Exhaust gas treatment module:

[0051] 61-Exhaust pipe; 62-Exhaust gas treatment device;

[0052] 7-Gas Sampling Module:

[0053] 71-Gas sampling container; 73-Fourth check valve; 74-Temperature and humidity sensor; 75-Gas chromatograph;

[0054] 8-Liquid Sampling Module:

[0055] 81-Liquid sampling container; 82-Liquid sampling tube. Detailed Implementation

[0056] To facilitate understanding and implementation of the present invention by those skilled in the art, the present invention will be further described in detail below with reference to embodiments. It should be understood that the embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0057] The high-temperature, high-pressure CO2 mineralization reaction apparatus containing impurities of the present invention will be described in detail below with reference to the accompanying drawings.

[0058] Example 1

[0059] The structure of the high-temperature, high-pressure impurity-containing mixed CO2 mineralization reaction device provided in this embodiment is as follows: Figure 1 As shown, it includes a gas supply module 1, a gas mixer 2, a mixed gas analysis module 4, a mineralization reactor 3, a vacuum module 5, a tail gas treatment module 6, a gas sampling module 7, and a liquid sampling module 8.

[0060] The gas supply module 1 includes a CO2 gas supply unit 11, an SO2 gas supply unit, and an NO2 gas supply unit. The CO2 gas supply unit 11 includes a CO2 cylinder 11a and a first supply pipe 11b. A first gas flow meter 11c is installed on the first supply pipe 11b, and one end of the first supply pipe 11b is connected to the outlet of the CO2 cylinder 11a. The SO2 gas supply unit includes an SO2 cylinder and a second supply pipe. A second gas flow meter is installed on the second supply pipe, and one end of the second supply pipe is connected to the outlet of the SO2 cylinder. The NO2 gas supply unit includes an NO2 cylinder and a third supply pipe. A third gas flow meter is installed on the third supply pipe, and one end of the third supply pipe is connected to the outlet of the NO2 cylinder.

[0061] The gas mixer includes a gas mixer housing 21, a primary spiral mixing pipe 22, a secondary mixing chamber 23, a stirring assembly, and a mixed gas output pipe 24. The gas mixer housing 21 is fixedly supported by a first bracket 25. The gas mixer housing 21 is a cylindrical body sealed at both ends, and has a cylindrical cavity. An inlet 21a and a first outlet 21b are respectively provided on one end face of the gas mixer housing 21, with the first outlet 21b located above the inlet 21a. The primary spiral mixing pipe 22 is spiral-shaped, with its spiral extension parallel to the axis of the gas mixer housing 21. The primary spiral mixing pipe 22 has multiple outlet holes evenly distributed along its length. The primary spiral mixing pipe 22 is fixed to the gas mixer housing 21 (the specific fixing structure is not shown), and is close to the inner wall of the gas mixer housing 21. The other ends of the first air supply pipe 11b, the second air supply pipe and the third air supply pipe are connected to the inlet of the air inlet 21a through a four-way valve. One end of the first-stage spiral mixing pipe 22 is connected to the outlet of the air inlet 21a, and the other end of the first-stage spiral mixing pipe 22 is closed.

[0062] The secondary mixing chamber 23 is a cylindrical body sealed at both ends. The secondary mixing chamber 23 has a cylindrical cavity, and multiple evenly distributed air inlets are provided on its sidewalls. The secondary mixing chamber 23 is located within the spiral space of the primary spiral mixing pipe 22, and is coaxial with the gas mixer housing 21. A second air outlet 23a is provided on the end face of the secondary mixing chamber 23 facing the first air outlet 21b. An air outlet pipe 26 is connected to the second air outlet 23a, and a second one-way valve 27 is provided on the air outlet pipe 26. One end of the air outlet pipe 26 is connected to the second air outlet 23a, and the air outlet pipe 26 passes through the first air outlet 21b.

[0063] The mixing assembly includes a mixing motor 28, a mixing shaft 29, and multiple mixing blades 210. The mixing motor 28 is located outside the gas mixer housing 21 and is fixed to the center of the other end face of the gas mixer housing 21. One end of the mixing shaft 29 is connected to the output shaft of the mixing motor 28. The mixing shaft 29 passes through the center of both end faces of the secondary mixing chamber 23 and is connected to both end faces of the secondary mixing chamber 23 via bearings. Multiple mixing blades 210 are located in the secondary mixing chamber 23, each mixing blade 210 is fixed to the mixing shaft 29, and the multiple mixing blades 210 are evenly distributed along the length of the mixing shaft 29.

[0064] The mineralization reactor includes a reactor shell 31 and a rock sample holder 315 for holding the rock sample to be mineralized. The reactor shell 31 has a cylindrical outer contour and is fixedly supported by a second bracket 32. The reactor shell 31 includes a top cover 31a and a reaction cylinder 31b, which are connected by threads, and an annular sealing ring is provided at the threaded connection between the top cover 31a and the reaction cylinder 31b. The reactor shell 31 is covered with a heat insulation and heating layer 33, which heats and insulates the mineralization reactor, reducing heat loss. The rock sample holder 315 is located inside the reaction cylinder 31b.

[0065] The top cover 31a has three functional interfaces 31a1, one of which is located in the center of the top of the top cover 31a, and the other two functional interfaces 31a1 are symmetrically arranged about the one in the center of the top of the top cover 31a. The functional interfaces 31a1 on both sides are respectively connected to a pressure gauge 34 and a temperature sensor 35. The pressure gauge 34 is used to monitor the pressure inside the reactor shell, and the temperature sensor 35 is used to monitor the temperature inside the reactor shell.

[0066] The bottom of the reaction cylinder 31b is relatively thick. The bottom of the reaction cylinder 31b is provided with an inverted conical gas injection port 31b1. The bottom of the tip of the gas injection port 31b1 is connected to a gas injection pipe 36. The gas injection pipe 36 penetrates the insulation layer 33 and the bottom of the reaction cylinder 31b, and the gas injection pipe 36 is fixed to the bottom of the reaction cylinder 31b. One end of the gas injection pipe 36 is connected to the bottom of the tip of the gas injection port 31b1.

[0067] One end of the mixed gas output pipe 24 is connected to the other end of the gas outlet pipe 26, and the other end of the mixed gas output pipe 24 is connected to the other end of the gas injection pipe 36 through a connector. A booster pump 211 is provided on the mixed gas output pipe 24.

[0068] An annular holding trough 37 is provided at the bottom edge of the reaction cylinder 31b, located around the gas injection port 31b1, and the holding trough 37 and the gas injection port 31b1 are coaxial. A water inlet / outlet pipe 38 is connected to the bottom of the holding trough 37, with one end connected to the holding trough 37. A first one-way valve 39 is provided on the water inlet / outlet pipe 38. A liquid simulating the environment of the rock sample, such as saline water or pure water, is injected into the holding trough 37. The saline water or pure water will evaporate during the mineralization process to provide a humidity environment.

[0069] The mineralization reactor 3 is equipped with a microporous filter plate 310, which is located at the top of the gas injection port 31b1 and seals the top of the gas injection port 31b1. The microporous filter plate 310 is fixed to the bottom of the reaction cylinder 31b by studs 312 evenly distributed along the circumference, and an annular pressure plate 311 is provided between the microporous filter plate 310 and the bottom of the reaction cylinder 31b. The top of the gas injection port 31b1 is provided with an annular sealing groove, and a sealing ring 313 is provided in the sealing groove. The sealing ring is located inside each stud 312.

[0070] The mixed gas analysis module 4 includes an analysis gas tube 41 and a gas analyzer 43. The two ends of the analysis gas tube 41 are connected to the mixed gas output tube 24 and the gas analyzer 43, respectively. The analysis gas tube 41 and the mixed gas output tube 24 are connected through a first tee 42, and the connection between the analysis gas tube 41 and the mixed gas output tube 24 is located between the booster pump 211 and the gas outlet tube 26. A fifth one-way valve 44 is provided on the analysis gas tube 41.

[0071] The vacuum module 5 includes a vacuum tube 51 and a vacuum pump 52. A second tee 314 is connected to a functional interface 31a1 located at the center of the top of the top cover. The main interface of the second tee 314 is connected to the functional interface 31a1 located at the center of the top of the top cover. One end of the vacuum tube 51 is connected to a branch interface of the second tee 314, and the other end of the vacuum tube 51 is connected to the vacuum pump 52. A third one-way valve 53 is provided on the vacuum tube 51.

[0072] The exhaust gas treatment module 6 includes an exhaust pipe 61 and an exhaust gas treatment device 62. One end of the exhaust pipe 61 is connected to the vacuum pipe 51, and the other end of the exhaust pipe 61 is connected to the exhaust gas treatment device 62.

[0073] The gas sampling module 7 includes a gas sampling container 71, a gas sampling tube, a temperature and humidity sensor 74, and a gas chromatograph 75. One end of the gas sampling tube is connected to another branch of the second three-way valve 314, and the other end of the gas sampling tube is connected to the gas sampling container 71. A fourth one-way valve 73 is provided on the gas sampling tube. The temperature and humidity sensor 74 is installed on the gas sampling container 71, and the gas chromatograph 75 is connected to the gas sampling container 71.

[0074] The liquid sampling module 8 includes a liquid sampling container 81 and a liquid sampling tube 82. One end of the liquid sampling tube 82 is snapped into the other end of the water inlet / outlet pipe 38, and the other end of the liquid sampling tube 82 is connected to the liquid sampling container 81.

[0075] The high-temperature, high-pressure impurity-containing mixed CO2 mineralization reaction method of the present invention will be described in detail below with reference to the above-described apparatus.

[0076] Example 2

[0077] 1. Place the rock sample to be mineralized on the rock sample holder 315, and then place the rock sample holder 315 on the microporous filter plate 310;

[0078] 2. Open CO2 cylinder 11, SO2 cylinder, NO2 cylinder, four-way valve, and stirring motor 28. Use the first flow meter 11c to control the flow rate of CO2 gas, the second flow meter to control the flow rate of SO2 gas, and the third flow meter to control the flow rate of NO2 gas. CO2, SO2, and NO2 gases enter the primary spiral mixing pipe 22 through the inlet 21a for primary mixing. The mixed gas in the primary spiral mixing pipe 22 enters the secondary mixing chamber 23 through the outlet, where it undergoes secondary mixing. The mixing is further enhanced by the stirring action of the stirring blades 210. After 20 minutes, close CO2 cylinder 11, SO2 cylinder, NO2 cylinder, and four-way valve.

[0079] 3. Open the second one-way valve 27 and the fifth one-way valve 44 to test the composition of the mixed gas after step 1. If the composition ratio of the mixed gas meets the requirements, turn off the stirring motor 28 to stop mixing. If the composition ratio of the mixed gas does not meet the requirements (error range greater than 5%), continue mixing until the mixed gas meets the test requirements, and then close the second one-way valve 27, the fifth one-way valve 44 and the stirring motor 28.

[0080] 4. Open the third check valve 53 and vacuum pump 52 to evacuate the reactor shell 31. After the reactor shell 31 reaches a vacuum state, close the third check valve 53 and vacuum pump 52.

[0081] 5. Open the first one-way valve 39 and inject saline water into the holding tank 37 through the water inlet / outlet pipe 38, then close the first one-way valve 39;

[0082] 6. Turn on the heat insulation and heating layer 33 to heat the reactor shell 31. After the reactor shell 31 reaches 80°C, keep it warm.

[0083] 7. Open the second one-way valve 27 and the booster pump 211 to inject mixed gas into the reactor shell 31. At the same time, use the mixed gas to pressurize the reactor shell 31. When the pressure inside the reactor shell 31 reaches 15 MPa, close the second control valve 27 and the booster pump 211.

[0084] 8. The mineralization reaction begins inside the reactor shell 31. During the mineralization reaction, if it is necessary to analyze the composition of the mixed gas and monitor the temperature and humidity, the fourth one-way valve 73 can be opened, and the mixed gas inside the reactor shell 31 enters the gas sampling container 71. The composition is analyzed by a gas chromatograph 75, and the temperature and humidity are monitored by a temperature and humidity sensor 74. If it is necessary to analyze the saline water in the placement tank 37 during the mineralization reaction, the liquid sampling pipe 82 can be connected to the inlet and outlet pipe 38, and then the first one-way valve 39 can be opened, allowing the saline water in the placement tank 37 to flow into the liquid sampling container 81 for sampling and analysis.

[0085] 9. After 7 days of mineralization, the mineralization reaction ends. The insulation and heating layer 33 is closed, and the third one-way valve 53 is opened. The tail gas generated by the mineralization reaction enters the tail gas treatment device 62 for treatment.

[0086] 10. Once the pressure inside the reactor shell 31 has dropped to atmospheric pressure, remove the mineralized rock sample.

Claims

1. A high-temperature, high-pressure CO2 mineralization reaction device containing impurities, characterized in that: It includes a gas supply module, a gas mixer, a mixed gas analysis module, a mineralization reactor, a vacuum module, and an exhaust gas treatment module; The gas supply module includes a CO2 gas supply unit and one or more impurity gas supply units; The gas mixer includes a gas mixer housing, a primary spiral mixing tube, and a mixed gas output tube. The primary spiral mixing tube is spiral-shaped and has multiple outlet holes evenly distributed along its length. The primary spiral mixing tube is fixed inside the gas mixer housing. The gas mixer housing has an inlet. The CO2 gas supply unit and each impurity gas supply unit are respectively connected to the inlet. One end of the primary spiral mixing tube is connected to the outlet of the inlet, and the other end of the primary spiral mixing tube is closed. The gas mixer housing has a first outlet. One end of the mixed gas output tube is connected to the first outlet. A booster pump is installed on the mixed gas output tube. The mixed gas analysis module is connected to the mixed gas output tube. The mineralization reactor includes a reactor shell and a rock sample support for placing the rock sample to be mineralized. The bottom of the reactor shell is equipped with an inverted conical gas injection port and an annular holding tank located around the gas injection port. The holding tank is connected to an injection and drainage pipe, one end of which is connected to the holding tank. The injection and drainage pipe is equipped with a first control valve to inject saline or pure water into the holding tank to simulate the liquid environment of the rock sample. The saline or pure water will evaporate during the mineralization process to provide a humidity environment. A pressure gauge and a temperature sensor are connected to the reactor shell. The other end of the mixed gas output pipe is connected to the gas injection port. A vacuum module and a tail gas treatment module are respectively connected to the reactor shell. The device integrates a water vapor evaporation control design. By controlling the content of liquid components, reaction temperature and pressure in the environmental simulation, it simulates the actual formation liquid water-water vapor coexistence environment and achieves water vapor evaporation control, thereby realistically reproducing the natural conditions of CO2 mineralization reaction.

2. The high-temperature, high-pressure CO2 mineralization reaction device containing impurities according to claim 1, characterized in that: The CO2 gas supply unit includes a CO2 cylinder and a first supply pipe. The first supply pipe is equipped with a first gas flow meter, and one end of the first supply pipe is connected to the outlet of the CO2 cylinder. There are two impurity gas supply units: an SO2 gas supply unit and a NO2 gas supply unit. The SO2 gas supply unit includes an SO2 cylinder and a second supply pipe. The second supply pipe is equipped with a second gas flow meter, and one end of the second supply pipe is connected to the outlet of the SO2 cylinder. The NO2 gas supply unit includes an NO2 cylinder and a third supply pipe. The third supply pipe is equipped with a third gas flow meter, and one end of the third supply pipe is connected to the outlet of the NO2 cylinder. The other ends of the first, second, and third supply pipes are connected to the inlet via a four-way valve.

3. The high-temperature, high-pressure CO2 mineralization reaction device containing impurities according to claim 1, characterized in that: The gas mixer further includes a secondary mixing chamber and a stirring assembly. The secondary mixing chamber is located within the spiral space of the primary spiral mixing tube. The secondary mixing chamber has multiple evenly distributed air inlets. The stirring assembly can stir the mixed gas in the secondary mixing chamber. The secondary mixing chamber has a second air outlet, and an air outlet pipe is connected to the second air outlet. One end of the air outlet pipe is connected to the second air outlet, and the air outlet pipe passes through the first air outlet. A second control valve is provided on the air outlet pipe, and one end of the mixed gas output pipe is connected to the other end of the air outlet pipe.

4. The high-temperature, high-pressure CO2 mineralization reaction apparatus containing impurities according to claim 3, characterized in that: The stirring assembly includes a stirring motor, a stirring shaft, and multiple stirring blades. The stirring motor is located outside the gas mixer housing and is fixed to one end face of the gas mixer housing. One end of the stirring shaft is connected to the output shaft of the stirring motor. The stirring shaft is parallel to the spiral extension direction of the primary spiral mixing pipe and passes through opposite sides of the secondary mixing chamber. The stirring shaft is rotatably connected to the secondary mixing chamber. Multiple stirring blades are located inside the secondary mixing chamber and are evenly distributed along the length of the stirring shaft.

5. The high-temperature, high-pressure CO2 mineralization reaction apparatus containing impurities according to claim 1, characterized in that: The mineralization reactor is equipped with a microporous filter plate, which seals the top of the container and the gas injection port. The microporous filter plate is fixed to the bottom of the reactor shell. The top of the gas injection port is provided with an annular sealing groove, and a sealing ring is provided in the sealing groove.

6. The high-temperature, high-pressure CO2 mineralization reaction apparatus containing impurities according to claim 1, characterized in that: The gas injection port tip is connected to a gas injection tube, one side of which is fixed to the bottom of the reactor shell, and one end of which is connected to the gas injection port.

7. The high-temperature, high-pressure CO2 mineralization reaction apparatus containing impurities according to claim 1, characterized in that: The vacuum module includes a vacuum tube and a vacuum pump. One end of the vacuum tube is connected to the reactor shell, and the other end of the vacuum tube is connected to the vacuum pump. A third control valve is provided on the vacuum tube.

8. The high-temperature, high-pressure CO2 mineralization reaction apparatus containing impurities according to claim 1, characterized in that: The exhaust gas treatment module includes an exhaust pipe and an exhaust gas treatment device. One end of the exhaust pipe is connected to the reactor shell, and the other end of the exhaust pipe is connected to the exhaust gas treatment device.

9. The high-temperature, high-pressure CO2 mineralization reaction apparatus containing impurities according to claim 1, characterized in that: It also includes a gas sampling module, which includes a gas sampling container, a gas sampling tube, a temperature and humidity sensor, and a gas chromatograph. The two ends of the gas sampling tube are connected to the reactor shell and the gas sampling container. A fourth control valve is provided on the gas sampling tube. The temperature and humidity sensor is installed on the gas sampling container. The gas chromatograph is connected to the gas sampling container.

10. The high-temperature, high-pressure CO2 mineralization reaction apparatus containing impurities according to claim 1, characterized in that: It also includes a liquid sampling module, which includes a liquid sampling container and a liquid sampling tube. One end of the liquid sampling tube is detachably connected to the other end of the inlet / outlet pipe, and the other end of the liquid sampling tube is connected to the liquid sampling container.

11. The high-temperature, high-pressure CO2 mineralization reaction apparatus containing impurities according to claim 1, characterized in that: The mixed gas analysis module includes an analysis gas tube and a gas analyzer. The analysis gas tube is equipped with a fifth control valve. The two ends of the analysis gas tube are connected to the mixed gas output tube and the gas analyzer, respectively. The connection between the analysis gas tube and the mixed gas output tube is located between the booster pump and the gas outlet tube.

12. A mineralization method based on the high-temperature, high-pressure mixed CO2 mineralization reaction device containing impurities as described in any one of claims 3-4, characterized in that... Includes the following steps: S1. Place the rock sample to be mineralized on the rock sample holder and put it into the reactor shell; S2. Turn on the CO2 gas supply unit and each impurity gas supply unit. CO2 gas and one or more impurity gases enter the gas mixer housing for mixing. When the amount of CO2 gas and each impurity gas entering the gas mixer housing reaches the set amount, turn off the CO2 gas supply unit and each impurity gas supply unit. After the CO2 gas and one or more impurity gases are fully mixed and homogeneous in the gas mixer housing, a mixed gas is obtained. S3. Turn on the mixed gas analysis module and the second control valve to test the composition of the mixed gas. If the composition ratio of the mixed gas meets the requirements, stop mixing. If the composition ratio of the mixed gas does not meet the requirements, continue mixing until the mixed gas meets the requirements. Then turn off the mixed gas analysis module and the second control valve. S4. Turn on the vacuum module to evacuate the reactor shell. Once the reactor shell is under vacuum, turn off the vacuum module. S5. Open the first control valve and inject the environmental simulation liquid into the holding tank through the injection and drainage pipe, then close the first control valve. S6. Heat the reactor shell and keep it warm after the reactor shell reaches the set temperature; S7. Open the second control valve and the booster pump to inject mixed gas into the reactor shell. At the same time, use the mixed gas to pressurize the reactor shell. When the pressure inside the reactor shell reaches the pressure required for the mineralization reaction, close the second control valve and the booster pump. S8. The mineralization reaction begins inside the reactor shell. After the mineralization reaction is completed, the heating of the reactor shell is stopped, and the tail gas treatment module is turned on to treat the tail gas generated by the mineralization reaction. S9. Once the pressure inside the reactor shell has dropped to atmospheric pressure, remove the rock sample.

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