CO2 dissolution mineralization reaction experiment system and method

By real-time monitoring of sample parameters in the reactor in the CO2 dissolution mineralization reaction experimental system, the problems of sample deterioration and unevenness in the prior art are solved, the accuracy of experimental results is improved, and an experimental environment consistent with the underground conditions of coal mines is achieved.

CN119915958APending Publication Date: 2025-05-02XIAN UNIV OF SCI & TECH
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Patent Information

Application Number
CN202510157924.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-13
Publication Date
2025-05-02

AI Technical Summary

Technical Problem

The dissolving mineralization reaction device in existing laboratories may cause the sample to deteriorate or be uneven during sample sampling and analysis, affecting the accuracy of experimental results, and cannot achieve a laboratory environment consistent with the underground conditions of coal mines.

Method used

Provide a CO2 dissolution mineralization reaction experimental system, including a reaction system, a gas supply system, a monitoring system and a sampling component. The system monitors the changes in the liquid phase ions, functional groups and pH parameters of the sample during CO2 mineralization in real time in the reactor, and uses the sampling component to directly transport the reaction liquid to the ion chromatograph and infrared spectrometer for detection.

Benefits of technology

Real-time monitoring of the changes in sample parameters in the reactor is achieved, the accuracy of experimental results is improved, and the experiment can be carried out closer to the underground conditions of the coal mine.

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Abstract

The invention discloses a CO2 dissolution mineralization reaction experiment system and method, and relates to the technical field of mineralization reaction experiments, and the CO2 dissolution mineralization reaction experiment system comprises a reaction system, a gas supply system, a monitoring system and a sampling assembly. A reaction kettle of the reaction system is used for providing an environment and a place for mineralizing CO2; the gas supply system is used for supplying CO2 into the reaction kettle and pressurizing; the monitoring system comprises an ion chromatograph, an infrared spectrometer and a pH sensor; the pH sensors are arranged in the reaction kettle; the pH sensor is immersed in the reaction liquid in the reaction kettle; the sampling assembly is used for sucking reaction liquid in the reaction kettle into the infrared spectrometer and the ion chromatograph in the experiment process. According to the invention, the change conditions of parameters such as main liquid phase ions, functional groups and pH of a sample in the CO2 mineralization process can be monitored in real time in the reaction kettle, so that the accuracy of an experimental result is improved.
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Description

Technical Field

[0001] The present invention relates to the technical field of mineralization reaction experiments, and in particular to a CO2 dissolution mineralization reaction experimental system and method. Background Art

[0002] my country's long-term energy consumption is mainly coal. In 2023, my country's coal consumption accounts for about 55.3% of my country's total energy consumption. In the process of coal resource mining, a large number of underground goafs have been formed, and the underground space resources have exceeded 15.6 billion m 3 At the same time, the global warming problem caused by carbon emissions has become increasingly prominent, accelerating the pace of low-carbon structural adjustment in the energy industry. CO2 emissions, as the main source of the greenhouse effect, are closely related to the use of fossil energy such as coal.

[0003] Carbon dioxide capture, utilization and storage (CCUS) technology is one of the necessary means of carbon emission reduction. Among them, CO2 mineral storage technology is a mode of storage by imitating the process of natural mineral weathering and absorbing CO2, using minerals containing calcium and magnesium ions to react with CO2 to convert into solid carbonate (such as CaCO3 / MgCO3). High-temperature and high-pressure reactors are important equipment for coal rock and solid waste mineralization CO2. They are mainly used to complete pressurized chemical reactions of materials under high temperature, high pressure and stirring conditions. At present, the dissolution mineralization reaction device in the laboratory first samples the reaction liquid before the reaction, samples it again after the dissolution mineralization reaction, and then puts the samples before and after the reaction into an ion chromatograph, infrared spectrometer and pH detector for characteristic analysis. These may cause the samples to deteriorate or become uneven before analysis, affecting the accuracy of the experimental results, failing to meet the required experimental requirements, and failing to truly achieve a laboratory environment consistent with the underground conditions of a coal mine. Summary of the invention

[0004] The purpose of the present invention is to provide a CO2 dissolution mineralization reaction experimental system and method to solve the problems existing in the above-mentioned prior art and improve the accuracy of the experimental results.

[0005] To achieve the above object, the present invention provides the following solutions:

[0006] The present invention provides a CO2 dissolution mineralization reaction experimental system, comprising: a reaction system, a gas supply system, a monitoring system and a sampling component. The reaction kettle of the reaction system is used to provide an environment and a place for mineralizing CO2; the gas supply system is used to supply CO2 and pressurize the reactor; the monitoring system comprises an ion chromatograph, an infrared spectrometer, and a pH sensor; the pH sensor is arranged in the reactor; two sampling components are provided, and the two sampling components are respectively arranged in the reactor, and the two sampling components can transport the reaction liquid in the reactor to the ion chromatograph and the infrared spectrometer respectively.

[0007] Preferably, it also includes a vacuum system; the vacuum system is used to evacuate the reaction kettle after the sample is placed.

[0008] Preferably, it also includes a control system, which controls the operation of the reaction system, the gas supply system, the monitoring system and the vacuum system.

[0009] Preferably, the gas supply system includes a CO2 gas tank and a pressurizing device; the gas outlets of the CO2 gas tank and the pressurizing device are both connected to the reactor, and the gas inlet of the pressurizing device is connected to the atmosphere outside the reactor.

[0010] Preferably, the reaction system comprises the reactor and a stirrer; the stirring head of the stirrer is arranged in the reactor.

[0011] Preferably, a heater is further included, and the heater is used to heat the sample, gas and reaction liquid in the reaction kettle.

[0012] Preferably, the sampling assembly includes a suction pump and a suction pipeline, one end of the suction pipeline is immersed in the reaction liquid, and the other end is connected to the inlet of the ion chromatograph or the infrared spectrometer, and the suction pump is arranged on the suction pipeline.

[0013] Preferably, the control system controls the suction pump to pump continuously or intermittently.

[0014] The present invention also provides a CO2 dissolution mineralization reaction experimental method, comprising:

[0015] Start the experiment;

[0016] During the experiment, the sampling component is used to draw the reaction liquid in the reactor into the infrared spectrometer and ion chromatograph for detection.

[0017] Preferably, before starting the experiment, it is necessary to prepare the sample, place the sample in the reactor and evacuate the reactor.

[0018] Compared with the prior art, the present invention has achieved the following technical effects:

[0019] The present invention can monitor the changes of parameters such as main liquid phase ions, functional groups and pH of the sample in real time during the CO2 mineralization process in the reactor, thereby improving the accuracy of the experimental results. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0021] Figure 1 A schematic diagram of the structure of a CO2 dissolution mineralization reaction experimental system provided in an embodiment of the present invention;

[0022] In the figure: 1-CO2 gas tank; 2-sampling component; 3-control system; 4-pH sensor; 5-boosting device; 6-gas supply system; 7-reaction system; 8-vacuum system; 9-monitoring system; 10-ion chromatograph; 11-infrared spectrometer. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0025] Combine the following Figure 1 , describing an embodiment of the present invention.

[0026] The present invention provides a CO2 dissolution mineralization reaction experimental system, comprising: a reaction system 7, a gas supply system 6, a monitoring system 9 and a sampling component 2. The reactor of the reaction system 7 is used to provide an environment and a place for mineralizing CO2; the gas supply system 6 is used to supply CO2 and pressurize the reactor; the monitoring system 9 comprises an ion chromatograph 10, an infrared spectrometer 11, and a pH sensor 4; the pH sensor 4 is arranged in the reactor; the pH sensor 4 is immersed in the reaction liquid in the reactor; two sampling components 2 are provided, and the two sampling components 2 are respectively arranged in the reactor, and the two sampling components 2 can transport the reaction liquid in the reactor to the ion chromatograph 10 and the infrared spectrometer 11 respectively.

[0027] The present invention can monitor the changes of parameters such as main liquid phase ions, functional groups and pH of the sample in real time during the CO2 mineralization process in the reactor, thereby improving the accuracy of the experimental results.

[0028] It can be understood that the above-mentioned real-time monitoring refers to detection during the experiment.

[0029] In some embodiments, the present invention further comprises a vacuum system 8; the vacuum system 8 is used to evacuate the reaction kettle after placing the sample.

[0030] The vacuum system 8 in this embodiment is used to provide the required vacuum environment for the experiment and to blow away the residual gas in the raw coal.

[0031] In some embodiments, the present invention further includes a control system 3 , which controls the operation of the reaction system 7 , the gas supply system 6 , the monitoring system 9 and the vacuum system 8 .

[0032] In some embodiments, the gas supply system 6 includes a CO2 gas tank 1 and a booster 5; the booster 5 is an air compressor, the gas outlets of the CO2 gas tank 1 and the booster 5 are both connected to the reactor, and the gas inlet of the booster 5 is connected to the atmosphere outside the reactor.

[0033] In this embodiment, the CO2 gas cylinder 1 provides CO2 into the reactor. When the pressure in the CO2 gas cylinder 1 is sufficient to maintain the high pressure in the reactor, there is no need to turn on the booster 5. After the CO2 gas cylinder 1 has worked for a certain period of time, the gas pressure therein becomes smaller and is insufficient to maintain the high pressure in the reactor. Then the booster 5 is controlled to perform auxiliary increase. Specifically, the booster 5 is a booster 5, which can pump external air into the reactor to increase the gas pressure in the reactor.

[0034] In some embodiments, the reaction system 7 includes a reaction kettle and a stirrer; the stirring head of the stirrer is disposed in the reaction kettle.

[0035] The stirrer in this embodiment is used to stir the sample and the reaction solution to make them uniformly mixed.

[0036] In some embodiments, the present invention further includes a heater, which is used to heat the sample, gas and reaction liquid in the reaction vessel.

[0037] In some embodiments, the sampling component 2 includes a suction pump and a suction pipeline, one end of the suction pipeline is immersed in the reaction liquid, and the other end is connected to the inlet of the ion chromatograph 10 or the infrared spectrometer 11, and the suction pump is arranged on the suction pipeline.

[0038] In some embodiments, the control system 3 controls the suction pump to pump continuously or intermittently.

[0039] The present invention also provides a CO2 dissolution mineralization reaction experimental method, comprising:

[0040] Start the experiment;

[0041] During the experiment, the sampling assembly 2 is used to draw the reaction liquid in the reactor during the experiment into the infrared spectrometer 11 and the ion chromatograph 10 for detection.

[0042] In some embodiments, before starting the experiment, it is necessary to prepare the sample, place the sample in the reaction vessel, and evacuate the reaction vessel.

[0043] The specific CO2 dissolution mineralization reaction experimental method is as follows.

[0044] 1. After sample preparation, place the sample in a sample basket and place it in the reactor.

[0045] 2. Add a certain amount of reaction liquid into the reactor according to the solid-liquid ratio set in the experiment.

[0046] 3. Before ventilation, use a vacuum to evacuate the reactor so that the pressure inside the reactor is displayed as -0.1MPa.

[0047] 4. Ventilation includes two steps. First, there is the CO2 gas passing step: first, introduce CO2 gas into the reactor. When the pressure in the CO2 gas tank 1 meets the experimental requirements, just use the CO2 gas tank 1 to pass CO2 gas into the reactor and make the reactor reach the set pressure. The pressure reading inside the reactor will continue to decrease due to the diffusion and dissolution of the gas. After the reading stabilizes, repeat the CO2 gas passing step; when the pressure in the CO2 gas tank 1 is not enough to meet the experimental needs, a pressure replenishing step is required: use the booster device 5 to pass air into the reactor to make the reactor reach the pressure required for the experiment. The reading inside the reactor will also continue to decrease due to diffusion and dissolution. When the pressure reading stabilizes, perform the pressure replenishing step again.

[0048] 5. After the ventilation operation, set the temperature and stirring speed on the touch interface of the reactor controller or on the computer.

[0049] 6. Turn on the monitoring system 9 to record the changes in the main chemical bonds, ion concentrations, pH and other parameters of the sample during the CO2 dissolution and mineralization reaction.

[0050] 7. Reaction liquid sampling. When sampling is required during the reaction process, slowly turn on the sampling switch of the reactor, then use a container to collect the reaction liquid at the sampling tube mouth, and then close the sampling switch. The pressure drop caused by the sampling process is compensated by the pressure compensation method during the repeated ventilation process.

[0051] 8. Sample unloading. After the reaction is completed, take out the sample and clean the reactor, then repeat the sample unloading operation for the next set of experiments.

[0052] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. At the same time, for those skilled in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

[0053] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. At the same time, for those skilled in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. A CO2 dissolution mineralization reaction experimental system, characterized in that: include: A reaction system, wherein the reactor of the reaction system is used to provide an environment and a place for mineralizing CO2; A gas supply system, used for supplying CO2 and pressurizing the reactor; and A monitoring system, the monitoring system comprising an ion chromatograph, an infrared spectrometer, and a pH sensor; the pH sensor is disposed in the reactor; The sampling components are provided with two, and the two sampling components are respectively arranged in the reactor, and the two sampling components can transport the reaction liquid in the reactor to the ion chromatograph and the infrared spectrometer respectively.

2. The CO2 dissolution mineralization reaction experimental system according to claim 1, characterized in that: It also includes a vacuum system; the vacuum system is used to evacuate the reaction kettle after the sample is placed.

3. The CO2 dissolution mineralization reaction experimental system according to claim 2, characterized in that: It also includes a control system, which controls the operation of the reaction system, the gas supply system, the monitoring system and the vacuum system.

4. The CO2 dissolution mineralization reaction experimental system according to claim 1, characterized in that: The gas supply system includes a CO2 gas tank and a pressurizing device; the gas outlets of the CO2 gas tank and the pressurizing device are both connected to the reactor, and the gas inlet of the pressurizing device is connected to the atmosphere outside the reactor.

5. The CO2 dissolution mineralization reaction experimental system according to claim 1, characterized in that: The reaction system comprises the reactor and a stirrer; the stirring head of the stirrer is arranged in the reactor.

6. The CO2 dissolution mineralization reaction experimental system according to claim 1, characterized in that: It also includes a heater, which is used to heat the sample, gas and reaction liquid in the reaction kettle.

7. The CO2 dissolution mineralization reaction experimental system according to claim 3, characterized in that: The sampling component comprises a suction pump and a suction pipeline, one end of the suction pipeline is immersed in the reaction liquid, and the other end is connected to the sampling port of the ion chromatograph or the infrared spectrometer, and the suction pump is arranged on the suction pipeline.

8. The CO2 dissolution mineralization reaction experimental system according to claim 7, characterized in that: The control system controls the suction pump to perform continuous suction or intermittent suction.

9. A CO2 dissolution mineralization reaction experimental method, characterized in that: include: Start the experiment; During the experiment, the sampling component is used to draw the reaction liquid in the reactor into the infrared spectrometer and ion chromatograph for detection.

10. The CO2 dissolution mineralization reaction experimental method according to claim 9, characterized in that: Before starting the experiment, it is necessary to prepare the sample, place the sample in the reactor, and evacuate the reactor.

Citation Information

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