High-temperature and high-pressure impurity-containing mixed CO2 mineralization reaction device and method

Abstract

The invention discloses a high-temperature high-pressure impurity-containing mixed CO2 mineralization reaction device and method.The high-temperature high-pressure impurity-containing mixed CO2 mineralization reaction device comprises a gas supply module, a gas mixer, a mixed gas analysis module, a mineralization reactor, a vacuumizing module and a tail gas treatment module, the gas supply module is used for providing CO2 gas and impurity gas, and the gas mixer is used for mixing the CO2 gas and the impurity gas; the mixed gas analysis module is used for judging whether CO2 gas and impurity gas are uniformly mixed or not, the mineralization reactor is used for simulating a mineralization reaction of a rock sample to be mineralized under the condition of the impurity CO2-containing mixed gas and environment simulation liquid, the vacuumizing module is used for vacuumizing the mineralization reactor, and the tail gas treatment module is used for treating tail gas generated by the mineralization reaction. The device capable of simulating the formation water vapor evaporation environment is developed, so that natural conditions can be reproduced more truly in an experiment, the performance of mineralization reaction under actual geological conditions can be better understood, and the research practicability is improved.

Description

Technical Field

[0001] The present invention belongs to CO 2 The field of mineralization technology specifically relates to a high-temperature, high-pressure, impurity-containing mixed CO 2 Mineralization reaction device and method. Background Art

[0002] Gas Mineralization is an emerging carbon dioxide capture and storage (CCS) technology. 2 It reacts with minerals to form stable solid carbonates, achieving permanent storage. In recent years, climate change issues have become increasingly serious, and the global demand for CO 2 The demand for emission control and reduction is increasing day by day, and CCS technology has received extensive attention and research in this context. 2 Aquifer storage is an important technical means to address climate change and reduce greenhouse gas emissions. Its basic principle is to capture CO 2 Injection into deep saline aquifers (i.e. groundwater layers containing salt water) for long-term storage and safe isolation. 2 - Saltwater-Rock Reactivity to CO 2 Monitoring and verification of saline aquifer storage projects is critical and requires rapid analysis through laboratory studies, especially for contaminated CO 2 Experiments with reactions of salt water and rocks.

[0003] In laboratory experiments, the impure CO 2 The mineralization reaction of mixed gas with rock and salt water is one of the key steps. However, the actual formation conditions usually involve high temperature and high pressure environment, and the mineral composition and salt water chemical composition in different formations are complex and varied. Therefore, how to accurately simulate these conditions in a laboratory or industrial environment and achieve the mineralization of impurity CO 2 Efficient mineralization reaction of gas and monitoring of water content in reaction gas have become the focus of technical research and development.

[0004] To overcome these challenges, researchers need to develop more advanced experimental equipment and techniques to simulate formation conditions at high temperature and pressure. At the same time, the design of the reactor is also crucial. The reactor is complex in design and difficult to operate, especially when dealing with impure gases, it is difficult to accurately 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 repeatability. At the same time, existing technologies are unable to effectively simulate the environment of formation water vapor evaporation, which limits the monitoring of gas water content during the mineralization reaction. Therefore, improving the design and control accuracy of the reaction system is the key to achieving efficient gas mineralization. Summary of the invention

[0005] In order to solve the problems existing in the above-mentioned prior art, the present invention provides a high-temperature, high-pressure, impurity-containing mixed CO 2 Mineralization reaction device and method. The present invention develops a device that can simulate the evaporation environment of water vapor in the formation so as to more realistically reproduce the natural conditions in the experiment. 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 purpose of the present invention is:

[0007] A high temperature and high pressure mixed CO 2 A mineralization reaction device, comprising a gas supply module, a gas mixer, a mixed gas analysis module, a mineralization reactor, a vacuum module and an exhaust gas treatment module;

[0008] Gas supply module including CO 2 a gas supply unit and one or more impurity gas supply units;

[0009] The gas mixer includes a gas mixer housing, a first-stage spiral gas mixing pipe and a mixed gas output pipe. The first-stage spiral gas mixing pipe is spiral-shaped and has a plurality of gas outlet holes evenly distributed along its length. The first-stage spiral gas mixing pipe is fixed in the gas mixer housing. The gas mixer housing is provided with an air inlet. 2 The gas supply unit and each impurity gas supply unit are respectively connected to the inlet of the gas inlet, one end of the first-stage spiral gas mixing pipe is connected to the outlet of the gas inlet, the other end of the first-stage spiral gas mixing pipe is closed, the gas mixer housing is provided with a first gas outlet, one end of the mixed gas output pipe is connected to the first gas outlet, a booster pump is provided on the mixed gas output pipe, and the mixed gas analysis module is connected to the mixed gas output pipe;

[0010] The mineralization reactor includes a reactor shell, a bracket for placing rock samples is arranged in the reactor shell, an inverted cone-shaped gas injection port is arranged at the bottom of the reactor shell, an annular holding groove is arranged at the bottom of the reactor shell, the holding groove is located outside the gas injection port, an injection and drainage pipe is connected to the holding groove, one end of the injection and drainage pipe is connected to the holding groove, a first control valve is arranged on the injection and drainage pipe, 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, and a vacuum module and an exhaust gas treatment module are respectively connected to the reactor shell.

[0011] The CO 2 Gas supply unit including CO 2 The gas cylinder and the first gas supply pipe are provided with a first gas flow meter, one end of the first gas supply pipe is connected to the CO 2The outlet of the gas cylinder is connected. There are two impurity gas supply units, namely SO 2 Gas supply unit and NO 2 Gas supply unit, SO 2 Gas supply unit including SO 2 The gas cylinder and the second gas supply pipe are provided with a second gas flow meter. One end of the second gas supply pipe is connected to the SO 2 Gas cylinder outlet connection, NO 2 Gas supply unit including NO 2 The gas cylinder and the third gas supply pipe are provided with a third gas flow meter. One end of the third gas supply pipe is connected to the NO 2 The gas cylinder outlet is connected, and the other ends of the first gas supply pipe, the second gas supply pipe and the third gas supply pipe are connected to the gas inlet through a four-way valve.

[0012] The gas mixer also includes a secondary gas mixing chamber and a stirring assembly. The secondary gas mixing chamber is located in the spiral space of the primary spiral gas mixing tube. The secondary gas mixing chamber is provided with a plurality of evenly distributed air inlet holes. The stirring assembly can stir the mixed gas in the secondary gas mixing chamber. The secondary gas mixing chamber is provided with a second gas outlet. The second gas outlet is connected to an gas outlet pipe. One end of the gas outlet pipe is connected to the second gas outlet. The gas outlet pipe runs through the first gas outlet. A second control valve is provided on the gas outlet pipe. One end of the mixed gas output pipe is connected to the other end of the gas outlet pipe.

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

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

[0015] The bottom of the tip of the gas injection port is connected with a gas injection pipe, one side of the gas injection pipe is fixed on the bottom of the reactor shell, and one end of the gas injection pipe is connected with the gas injection port.

[0016] The vacuum module comprises 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 arranged on the vacuum tube.

[0017] It also includes a tail gas treatment module, which includes a tail gas pipe and a tail gas treatment device. One end of the tail gas pipe is connected to the reactor shell, and the other end of the tail gas pipe is connected to the tail 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. Both 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 injection and discharge pipe, and the other end of the liquid sampling tube is connected to the liquid sampling container.

[0020] The mixed gas analysis module comprises an analysis gas pipe and a gas analyzer. The analysis gas pipe is provided with a fifth control valve. Both ends of the analysis gas pipe are respectively connected to the mixed gas output pipe and the gas analyzer. The connection between the analysis gas pipe and the mixed gas output pipe is located between the booster pump and the gas outlet pipe.

[0021] A high temperature and high pressure impurity-containing mixed CO 2 The mineralization method of the mineralization reaction device comprises the following steps:

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

[0023] S2. Turn on CO 2 Gas supply unit and each impurity gas supply unit, CO 2 Gas and one or more impurity gases enter the gas mixer shell for mixing. 2 When the amount of gas and impurity gases entering the gas mixer shell reaches the set amount, the CO 2 Gas supply unit and each impurity gas supply unit, CO 2 After the gas and one or more impurity gases are fully and evenly mixed in the gas mixer shell, a mixed gas is obtained;

[0024] S3, opening the mixed gas analysis module and the second control valve, testing the composition of the mixed gas, if the composition ratio of the mixed gas meets the requirements, then stopping the mixing, if the composition ratio of the mixed gas does not meet the requirements, then continuing the mixing until the mixed gas meets the test requirements, then closing the mixed gas analysis module and the second control valve;

[0025] S4, turning on the vacuum pumping module to evacuate the reactor shell, and after the reactor shell reaches a vacuum state, turning off the vacuum pumping module;

[0026] S5, opening the first control valve, injecting the environmental simulation liquid into the holding tank through the injection and drainage pipe, and then closing the first control valve;

[0027] S6, heating the reactor shell, and keeping the reactor shell warm after reaching the set temperature;

[0028] S7, open the second control valve and the booster pump, inject the mixed gas into the reactor shell, and pressurize the reactor shell with the mixed gas. When the pressure in the reactor shell reaches the pressure required for the mineralization reaction, close the second control valve and the booster pump;

[0029] S8, a mineralization reaction begins in 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;

[0030] S9. When the pressure inside the reactor shell drops to atmospheric pressure, take out 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 enters the gas sampling container, and is analyzed by a gas chromatograph and monitored by a temperature and humidity sensor; if it is necessary to perform liquid analysis on the environmental simulation liquid placed in the tank during the mineralization reaction, the first control valve is opened, and the environmental simulation liquid in the tank flows into the liquid sampling container.

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

[0033] 1. The gas mixer of the present invention has good mixing effect, making CO 2 The impurity gas is mixed more evenly, and the gas mixer of the present invention can mix different types of gases to meet various reaction requirements. This adaptability enables the system to play a role in different industrial applications and meet diverse laboratory / market requirements.

[0034] 2. The present invention can simulate pure CO 2 The mineralization reaction can also simulate the actual industrial emission of CO 2 Tail gas (CO 2 The mineralization reaction of various impurities (such as sulfides, nitrogen oxides, hydrocarbons, etc.) in the tail gas has expanded the scope of application and has good research and development prospects.

[0035] 3. The present invention includes a design for water vapor evaporation control, which simulates the actual formation liquid water-water vapor coexistence environment and realizes water vapor evaporation control by controlling the content of environmental simulation liquid components, reaction temperature and pressure, thereby truly reproducing CO 2The natural conditions of mineralization reaction improve the simulated CO 2 The accuracy and reliability of the mineralization reaction experimental results have improved the CO 2 The value of mineralization reaction research.

[0036] 4. The present invention can not only realize gas mixing and mineralization reaction, but also can sample, analyze and test the mixed gas and environmental simulation liquid in the mineralization reaction process. This multifunctionality enables the device of the present invention to flexibly respond to different needs during the experiment, thereby improving the wide application of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 High temperature and high pressure mixed CO 2 Schematic diagram of the structure of the mineralization reaction device.

[0038] Figure 2 Schematic diagram of the structure of the gas mixer.

[0039] Figure 3 Schematic diagram of the structure of the mineralization reactor.

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

[0041] 11-CO 2 Gas supply unit: 11a-CO 2 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 spiral gas mixing pipe; 23-secondary gas mixing chamber: 23a-second air outlet; 24-mixed gas output pipe; 25-first bracket; 26-air outlet pipe; 27-second one-way valve; 28 stirring motor; 29-stirring shaft; 210-stirring fan blade; 211-boosting pump;

[0044] 3-Mineralization reactor:

[0045] 31-reactor shell: 31a-top cover: 31a1-functional interface; 31b-reaction cylinder: 31b1-gas injection port; 32-second bracket; 33-insulation layer; 34-pressure gauge; 35-temperature sensor; 36-gas injection pipe; 37-holding tank; 38-injection and drainage pipe; 39-first one-way valve; 310-microporous filter plate; 311-annular pressing sheet; 312-stud; 313-sealing ring; 314-first three-way; 315-rock sample bracket;

[0046] 4-Mixed gas analysis module:

[0047] 41-analysis gas pipe; 42-second three-way connection; 43-gas analyzer; 44-fifth one-way valve;

[0048] 5-Vacuum module:

[0049] 51- vacuum tube; 52- vacuum pump; 53- third one-way valve;

[0050] 6- Exhaust treatment module:

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

[0052] 7-Gas sampling module:

[0053] 71-gas sampling container; 72-gas sampling tube; 73-fourth one-way valve; 74-temperature and humidity sensor; 75-gas chromatograph;

[0054] 8-Liquid sampling module:

[0055] 81-Liquid sampling container; 82-Liquid sampling tube. DETAILED DESCRIPTION

[0056] In order to facilitate those skilled in the art to understand and implement the present invention, the present invention is further described in detail below in conjunction with embodiments. It should be understood that the implementation examples described herein are only used to illustrate and explain the present invention and are not used to limit the present invention.

[0057] The high temperature and high pressure mixed CO containing impurities of the present invention is described below in conjunction with the accompanying drawings. 2 The mineralization reaction device is described in detail.

[0058] Example 1

[0059] The high temperature and high pressure impurity-containing mixed CO provided in this embodiment 2 The structure of the mineralization reaction device 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] Gas supply module 1 includes CO 2 Gas supply unit 11, SO 2 Gas supply unit and NO 2 Gas supply unit. CO 2 The gas supply unit 11 includes CO 2 The gas cylinder 11a and the first gas supply pipe 11b are provided with a first gas flow meter 11c. One end of the first gas supply pipe 11b is connected to the CO 2 Gas cylinder 11a outlet connection. SO 2 Gas supply unit including SO2 The gas cylinder and the second gas supply pipe are provided with a second gas flow meter. One end of the second gas supply pipe is connected to the SO 2 Gas cylinder outlet connection. NO 2 Gas supply unit including NO 2 The gas cylinder and the third gas supply pipe are provided with a third gas flow meter. One end of the third gas supply pipe is connected to the NO 2 Gas cylinder outlet connection.

[0061] The gas mixer comprises 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, and 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 the gas mixer housing 21 has a cylindrical cavity. An air inlet 21a and a first air outlet 21b are respectively provided on one end surface of the gas mixer housing 21, and the first air outlet 21b is located above the air inlet 21a. The primary spiral mixing pipe 22 is spiral-shaped, and the spiral extension of the primary spiral mixing pipe 22 is parallel to the axis of the gas mixer housing 21. The primary spiral mixing pipe 22 is provided with a plurality of air outlets evenly distributed along its length. The primary spiral mixing pipe 22 is fixed on the gas mixer housing 21 (the specific fixing structure is not shown), and the primary spiral mixing pipe 22 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 gas mixing chamber 23 is a cylindrical body sealed at both ends. The secondary gas mixing chamber 23 has a cylindrical cavity, and a plurality of evenly distributed air inlet holes are arranged on the side wall of the secondary gas mixing chamber 23. The secondary gas mixing chamber 23 is located in the spiral space of the primary spiral gas mixing pipe 22, and the secondary gas mixing chamber 23 is coaxial with the gas mixer housing 21. A second gas outlet 23a is arranged on the end surface of the secondary gas mixing chamber 23 facing the first gas outlet 21b, and an air outlet pipe 26 is connected to the second gas outlet 23a, and a second one-way valve 27 is arranged on the air outlet pipe 26. One end of the air outlet pipe 26 is connected to the second gas outlet 23a, and the air outlet pipe 26 runs through the first gas outlet 21b.

[0063] The stirring assembly includes a stirring motor 28, a stirring shaft 29 and a plurality of stirring blades 210. The stirring motor 28 is located outside the gas mixer housing 21, and the stirring motor 28 is fixed to the center of the other end surface of the gas mixer housing 21. One end of the stirring shaft 29 is connected to the output shaft of the stirring motor 28, and the stirring shaft 29 passes through the centers of the two end surfaces of the secondary gas mixing chamber 23 respectively, and the stirring shaft 29 is connected to the two end surfaces of the secondary gas mixing chamber 23 respectively through bearings. A plurality of stirring blades 210 are located in the secondary gas mixing chamber 23, each stirring blade 210 is fixed to the stirring shaft 29, and the plurality of stirring blades 210 are evenly distributed along the length direction of the stirring shaft 29.

[0064] The mineralization reactor includes a reactor shell 31 and a rock sample holder 315 for placing the rock sample to be mineralized. The outer contour of the reactor shell 31 is cylindrical, and the reactor shell 31 is fixedly supported by a second holder 32. The reactor shell 31 includes a top cover 31a and a reaction cylinder 31b. The top cover 31a and the reaction cylinder 31b 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 wrapped with a heat-insulating heating layer 33, and the mineralization reactor is heated and insulated by the heat-insulating heating layer 33 to reduce heat loss. A holder 315 for placing the rock sample is provided in the reaction cylinder 31b.

[0065] Three functional interfaces 31a1 are provided on the top of the top cover 31a, one of which is located at the center of the top of the top cover 31a, and the other two functional interfaces 31a1 are symmetrically arranged about the functional interface 31a1 located at the center of the top of the top cover 31a. The functional interfaces 31a1 located 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 in the reactor shell, and the temperature sensor 35 is used to monitor the temperature in the reactor shell.

[0066] The bottom of the reaction cylinder 31b is relatively thick, and an inverted cone-shaped gas injection port 31b1 is provided at the bottom of the reaction cylinder 31b. The bottom of the tip of the gas injection port 31b1 is connected to a gas injection pipe 36. The gas injection pipe 36 passes through the insulation layer 33 and the bottom of the reaction cylinder 31b, and the gas injection pipe 36 is fixed on the bottom of the reaction cylinder 31b, and 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 via a joint. A booster pump 211 is provided on the mixed gas output pipe 24 .

[0068] An annular holding groove 37 is provided at the bottom edge of the reaction cylinder 31b. The holding groove 37 is located outside the gas injection port 31b1, and the holding groove 37 and the gas injection port 31b1 are coaxial. An injection and drainage pipe 38 is connected to the bottom of the holding groove 37. One end of the injection and drainage pipe 38 is connected to the holding groove 37. A first one-way valve 39 is provided on the injection and drainage pipe 38. Salt water or pure water or other liquids simulating the environment of the rock sample are injected into the holding groove 37. The salt water or pure water will evaporate during the mineralization process to provide a humidity environment.

[0069] A microporous filter plate 310 is provided in the mineralization reactor 3. The microporous filter plate 310 is located at the top of the gas injection port 31b1, and the microporous filter plate 310 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 circumferential direction, and an annular pressing plate 311 is provided between the microporous filter plate 310 and the bottom of the reaction cylinder 31b. An annular sealing ring groove is provided at the top of the gas injection port 31b1, and a sealing ring 313 is provided in the sealing ring groove, and the sealing ring is located inside each stud 312.

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

[0071] The vacuum module 5 includes a vacuum tube 51 and a vacuum pump 52. The functional interface 31a1 located at the center of the top of the top cover is connected to the second tee 314. 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 gas pipe 61 and an exhaust gas treatment device 62 . One end of the exhaust gas pipe 61 is connected to the vacuum pipe 51 , and the other end of the exhaust gas 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 72, a temperature and humidity sensor 74, and a gas chromatograph 75. One end of the gas sampling tube 72 is connected to the other branch interface of the second three-way 314, and the other end of the gas sampling tube 72 is connected to the gas sampling container 71. The gas sampling tube 72 is provided with a fourth one-way valve 73. 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 clamped with the other end of the injection and drainage pipe 38 , and the other end of the liquid sampling tube 82 is connected to the liquid sampling container 81 .

[0075] Next, the high temperature and high pressure impurity mixed CO of the present invention is combined with the above-mentioned device. 2 The method of the mineralization reaction is described in detail.

[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. Turn on CO 2 Gas cylinder 11, SO 2 Gas cylinder, NO 2 The gas cylinder, the four-way valve and the stirring motor 28 are used to control the CO 2 The gas flow rate is controlled by a second flow meter SO 2 The gas flow rate is controlled by a third flow meter. 2 Gas flow rate, CO 2 Gas, SO 2 Gas and NO 2 The gas enters the primary spiral mixing tube 22 through the air inlet 21a for primary mixing. The mixed gas in the primary spiral mixing tube 22 enters the secondary mixing chamber 23 through the air outlet. The mixed gas is mixed in the secondary mixing chamber 23 and is mixed more evenly under the stirring action of the stirring blades 210. After 20 minutes, turn off the CO 2 Gas cylinder 11, SO 2 Gas cylinder, NO 2 Gas 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 mixed in 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 (the error range is 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 one-way valve 53 and the vacuum pump 52 to evacuate the reactor housing 31. After the reactor housing 31 reaches a vacuum state, close the third one-way valve 53 and the vacuum pump 52;

[0081] 5. Open the first one-way valve 39, inject salt water into the storage tank 37 through the injection and discharge pipe 38, and then close the first one-way valve 39;

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

[0083] 7. Open the second check valve 27 and the booster pump 211, inject the mixed gas into the reactor shell 31, and pressurize the reactor shell 31 with the mixed gas. When the pressure in the reactor shell 31 reaches 15 MPa, close the second control valve 27 and the booster pump 211;

[0084] 8. The mineralization reaction begins in 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 during the mineralization reaction, the fourth one-way valve 73 can be opened, and the mixed gas in the reactor shell 31 enters the gas sampling container 71, and the composition is analyzed by the gas chromatograph 75 and the temperature and humidity are monitored by the temperature and humidity sensor 74. If it is necessary to analyze the salt water in the placement tank 37 during the mineralization reaction, the liquid sampling tube 82 can be connected to the injection and drainage pipe 38, and then the first one-way valve 39 is opened, and the salt water in the placement tank 37 flows into the liquid sampling container 81, and then sampling and analysis are performed.

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

[0086] 10. When the pressure in the reactor shell 31 drops to atmospheric pressure, take out the mineralized rock sample.

Claims

1. A high temperature and high pressure impurity mixed CO2 mineralization reaction device, 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 comprises a gas mixer housing, a first-stage spiral gas mixing pipe and a mixed gas output pipe. The first-stage spiral gas mixing pipe is spiral-shaped and is provided with a plurality of gas outlet holes evenly distributed along its length direction. The first-stage spiral gas mixing pipe is fixed in the gas mixer housing. An air inlet is provided on the gas mixer housing. The CO2 gas supply unit and each impurity gas supply unit are respectively connected to the air inlet inlet. One end of the first-stage spiral gas mixing pipe is connected to the air inlet outlet. The other end of the first-stage spiral gas mixing pipe is closed. The gas mixer housing is provided with a first air outlet. One end of the mixed gas output pipe is connected to the first air outlet. A booster pump is provided on the mixed gas output pipe. The mixed gas analysis module is connected to the mixed gas output pipe. The mineralization reactor includes a reactor shell, an inverted cone-shaped gas injection port is provided at the bottom of the reactor shell, an annular holding tank is provided at the bottom of the reactor shell, the holding tank is located outside the gas injection port, an injection and drainage pipe is connected to the holding tank, one end of the injection and drainage pipe is connected to the holding tank, a first control valve is provided on the injection and drainage pipe, 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, and a vacuum module and an exhaust gas treatment module are respectively connected to the reactor shell.

2. The high-temperature and high-pressure impurity-containing mixed CO2 mineralization reaction device according to claim 1 is characterized in that: The CO2 gas supply unit includes a CO2 gas cylinder and a first gas supply pipe, the first gas supply pipe is provided with a first gas flowmeter, one end of the first gas supply pipe is connected to the outlet of the CO2 gas cylinder, there are two impurity gas supply units, the two impurity gas supply units are a SO2 gas supply unit and a NO2 gas supply unit, the SO2 gas supply unit includes a SO2 gas cylinder and a second gas supply pipe, the second gas supply pipe is provided with a second gas flowmeter, one end of the second gas supply pipe is connected to the outlet of the SO2 gas cylinder, the NO2 gas supply unit includes a NO2 gas cylinder and a third gas supply pipe, the third gas supply pipe is provided with a third gas flowmeter, one end of the third gas supply pipe is connected to the outlet of the NO2 gas cylinder, and the other ends of the first gas supply pipe, the second gas supply pipe and the third gas supply pipe are connected to the air inlet through a four-way valve.

3. The high temperature and high pressure impurity-containing mixed CO2 mineralization reaction device according to claim 1 is characterized in that: The gas mixer also includes a secondary gas mixing chamber and a stirring assembly. The secondary gas mixing chamber is located in the spiral space of the primary spiral gas mixing tube. The secondary gas mixing chamber is provided with a plurality of evenly distributed air inlet holes. The stirring assembly can stir the mixed gas in the secondary gas mixing chamber. The secondary gas mixing chamber is provided with a second gas outlet. The second gas outlet is connected to an gas outlet pipe. One end of the gas outlet pipe is connected to the second gas outlet. The gas outlet pipe runs through the first gas outlet. A second control valve is provided on the gas outlet pipe. One end of the mixed gas output pipe is connected to the other end of the gas outlet pipe.

4. The high-temperature and high-pressure impurity-containing mixed CO2 mineralization reaction device according to claim 3 is characterized in that: The stirring assembly includes a stirring motor, a stirring shaft and a plurality of stirring blades. The stirring motor is located outside the gas mixer housing, and the stirring motor is fixed to one end surface 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 tube. The stirring shaft passes through the opposite sides of the secondary mixing chamber respectively. The stirring shaft is rotatably connected to the secondary mixing chamber. The plurality of stirring blades are located in the secondary mixing chamber, and the plurality of stirring blades are evenly distributed along the length direction of the stirring shaft.

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

6. The high temperature and high pressure impurity-containing mixed CO2 mineralization reaction device according to claim 1 is characterized in that: The bottom of the tip of the gas injection port is connected with a gas injection pipe, one side of the gas injection pipe is fixed on the bottom of the reactor shell, and one end of the gas injection pipe is connected with the gas injection port.

7. The high temperature and high pressure impurity-containing mixed CO2 mineralization reaction device according to claim 1 is characterized in that: The vacuum module comprises 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 arranged on the vacuum tube.

8. The high-temperature and high-pressure impurity-containing mixed CO2 mineralization reaction device according to claim 1 is characterized in that: The tail gas treatment module comprises a tail gas pipe and a tail gas treatment device, one end of the tail gas pipe is communicated with the reactor shell, and the other end of the tail gas pipe is connected to the tail gas treatment device.

9. The high temperature and high pressure impurity-containing mixed CO2 mineralization reaction device 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. Both 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 and high pressure impurity-containing mixed CO2 mineralization reaction device 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 injection and discharge pipe, and the other end of the liquid sampling tube is connected to the liquid sampling container.

11. The high temperature and high pressure impurity-containing mixed CO2 mineralization reaction device according to claim 1, characterized in that: The mixed gas analysis module comprises an analysis gas pipe and a gas analyzer. The analysis gas pipe is provided with a fifth control valve. Both ends of the analysis gas pipe are respectively connected to the mixed gas output pipe and the gas analyzer. The connection between the analysis gas pipe and the mixed gas output pipe is located between the booster pump and the gas outlet pipe.

12. A mineralization method based on the high temperature and high pressure impurity mixed CO2 mineralization reaction device according to any one of claims 1 to 11, characterized in that The steps include: S1. Place the rock sample to be mineralized into the reactor shell; S2, open the CO2 gas supply unit and each impurity gas supply unit, and the CO2 gas and one or more impurity gases enter the gas mixer shell for mixing. When the amount of CO2 gas and each impurity gas entering the gas mixer shell reaches a set amount, close the CO2 gas supply unit and each impurity gas supply unit, and the CO2 gas and one or more impurity gases are fully mixed in the gas mixer shell to obtain a mixed gas; S3, opening the mixed gas analysis module and the second control valve, testing the composition of the mixed gas, if the composition ratio of the mixed gas meets the requirements, then stopping the mixing, if the composition ratio of the mixed gas does not meet the requirements, then continuing the mixing until the mixed gas meets the requirements, then closing the mixed gas analysis module and the second control valve; S4, turning on the vacuum pumping module to evacuate the reactor shell, and after the reactor shell reaches a vacuum state, turning off the vacuum pumping module; S5, opening the first control valve, injecting the environmental simulation liquid into the holding tank through the injection and drainage pipe, and then closing the first control valve; S6, heating the reactor shell, and keeping the reactor shell warm after reaching the set temperature; S7, open the second control valve and the booster pump, inject the mixed gas into the reactor shell, and pressurize the reactor shell with the mixed gas. When the pressure in the reactor shell reaches the pressure required for the mineralization reaction, close the second control valve and the booster pump; S8, a mineralization reaction begins in 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. When the pressure inside the reactor shell drops to atmospheric pressure, take out the rock sample.

13. The mineralization method according to claim 12, characterized in that: 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 enters the gas sampling container, and is analyzed by a gas chromatograph and monitored by a temperature and humidity sensor; if it is necessary to perform liquid analysis on the environmental simulation liquid placed in the tank during the mineralization reaction, the first control valve is opened, and the environmental simulation liquid in the tank flows into the liquid sampling container.

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