A continuous sampling double-compartment structure reaction device and method
By designing a dual-chamber structure reaction device capable of continuous sampling, the problems of reaction disturbance and insufficient high-pressure sealing performance in the carbon dioxide mineralization reaction device during sampling were solved, realizing efficient and accurate multiphase sample sampling and improving the reliability and accuracy of experimental data.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- SHENZHEN UNIV
- Filing Date
- 2026-04-03
- Publication Date
- 2026-06-09
AI Technical Summary
Existing carbon dioxide mineralization reaction devices are prone to reaction disturbances during the sampling process, affecting the reliability and accuracy of experimental data, and also suffer from insufficient high-pressure sealing performance.
Design a dual-chamber reaction device for continuous sampling, including a reaction chamber and a sampling chamber, equipped with gate valves, a core pushing system, a liquid injection and gas injection system, a liquid phase and gas phase acquisition system, and a monitoring system. The control system maintains the pressure stability in the reaction chamber, enabling multiphase sample sampling under pressure-free conditions.
Maintaining high pressure during sampling reduces the impact on the reaction chamber environment, enabling precise and efficient sampling of multiphase samples, improving sampling reliability and data accuracy, and meeting the requirements of high-pressure carbon dioxide mineralization reaction experiments.
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Figure CN121944916B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of high-pressure mineralization reaction experimental equipment technology, and in particular to a dual-chamber structure reaction device and method capable of continuous sampling. Background Technology
[0002] With the acceleration of global industrialization, the demand for global carbon emission reduction is becoming increasingly urgent. Carbon dioxide mineralization technology, due to its combined value in carbon sequestration and resource recycling, has become a research hotspot in the fields of addressing climate change and efficient resource utilization. In experimental research on carbon dioxide mineralization technology, obtaining data from liquid, gas, and solid phase samples within the reaction system to support the explanation of reaction mechanisms, analysis of kinetic characteristics, and optimization of process parameters is crucial for promoting the technology from the laboratory to industrial application.
[0003] However, existing carbon dioxide mineralization reaction devices typically depressurize first during the sampling process to connect the sampling container or open the sampling port before removing the sample. This method disrupts the pressure balance of the reaction system, causing reaction disturbances and easily introducing external impurities to contaminate the sample. Consequently, the authenticity, accuracy, and repeatability of the obtained experimental data are difficult to guarantee, making the experimental results unsuitable for the high-pressure operating conditions commonly required for mineralization reactions.
[0004] Therefore, existing technologies still need to be improved and developed. Summary of the Invention
[0005] In view of the shortcomings of the prior art, the purpose of this invention is to provide a dual-compartment reaction device and method for continuous sampling, which aims to solve the problem that sampling operations in existing carbon dioxide mineralization technologies are prone to causing reaction disturbances and affecting the reliability of experimental data.
[0006] The technical solution of the present invention is as follows:
[0007] A dual-compartment reaction device capable of continuous sampling, comprising:
[0008] Reaction chamber;
[0009] A sampling chamber is located at the top of the reaction chamber; a gate valve is installed between the sampling chamber and the reaction chamber;
[0010] The core delivery system is vertically mounted inside the reaction chamber and is used to hold the core to be reacted and to deliver the core to the sampling chamber.
[0011] Both the liquid injection system and the gas injection system are connected to the reaction chamber; the liquid injection system is used to inject a solution into the reaction chamber; the gas injection system is used to inject experimental gas into the reaction chamber.
[0012] Both the liquid phase acquisition system and the gas phase acquisition system are connected to the reaction chamber; the liquid phase acquisition system is used to acquire liquid phase samples; the gas phase acquisition system is used to acquire gas phase samples.
[0013] A monitoring system, connected to the reaction chamber, is used to collect operating parameters within the reaction chamber;
[0014] The control system is electrically connected to the core delivery system, the liquid injection system, the gas injection system, the liquid phase acquisition system, the gas phase acquisition system, and the monitoring system, and is used to maintain the pressure value inside the reaction chamber.
[0015] The continuously sampling dual-chamber reaction device includes a reaction chamber comprising a constant-temperature water bath and a reaction vessel placed within the water bath. The reaction vessel contains a bottom chamber and a reaction chamber. The liquid injection system, gas injection system, liquid phase acquisition system, gas phase acquisition system, and monitoring system are all connected to the reaction vessel and extend into the reaction chamber. A sampling channel communicating with the reaction chamber is provided at the top of the reaction vessel, and this sampling channel is used to connect to the sampling chamber. A gate valve is located on the reaction vessel for opening and closing the sampling channel. The core delivery system is located in the bottom chamber, below the reaction chamber.
[0016] The bottom of the reaction chamber is provided with a connecting hole, which is directly opposite the sampling channel; the core pushing system passes through the connecting hole and is inserted into the reaction chamber to hold the core to be reacted and push the core to the sampling chamber.
[0017] The continuously sampling dual-chamber structure reaction device, wherein the reaction chamber further includes a core holder, which extends longitudinally and is rotatably mounted on the reaction vessel;
[0018] The core holder is equipped with a rotary valve at its top, which is used to drive the core holder to rotate.
[0019] The bottom end of the core holder extends into the reaction chamber and is provided with multiple layers of staggered fixing frames; the fixing frames are provided with multiple ring-shaped locking holes, the diameter of which is equal to the diameter of the sampling channel, so as to constrain the core to be reacted inserted into the reaction chamber.
[0020] The continuously sampling dual-compartment reaction device is provided with multiple sampling channels, which are arranged in a ring around the circumference of the reaction vessel.
[0021] Multiple gate valves are provided, and one gate valve is provided at each of the sampling channels;
[0022] The sampling chambers are provided in multiple ways, and each sampling channel is connected to one of the sampling chambers.
[0023] The continuously sampling dual-chamber structure reaction device, wherein the core pushing system includes a lifter and a pushing support, the lifter is located in the bottom chamber and the movable end of the lifter can move toward the connecting hole; the pushing support is located at the movable end of the lifter;
[0024] The diameter of the pusher support is equal to the diameter of the connecting hole.
[0025] The aforementioned dual-compartment reaction device capable of continuous sampling includes a first viewing window on the reaction compartment and a second viewing window on the sampling compartment.
[0026] The continuously sampling dual-chamber reaction device includes an injection system comprising an injection pump and a storage bottle, wherein the storage bottle is used to store the experimental solution; one end of the injection pump is connected to the storage bottle and the other end is connected to the reaction chamber for injecting the solution into the reaction chamber.
[0027] The gas injection system includes a gas injection pump and a gas cylinder, the gas cylinder being used to store carbon dioxide gas; one end of the gas injection pump is connected to the gas cylinder, and the other end is connected to the reaction chamber, for injecting carbon dioxide gas into the reaction chamber.
[0028] The continuously sampling dual-chamber reaction device includes a liquid phase acquisition system comprising a drain pipe connected to the reaction chamber, a back pressure valve, a back pressure pump, and a back pressure replenishment bottle sequentially arranged on the drain pipe, and a sampling bottle connected to the back pressure valve; the back pressure valve is used to open or close the drain pipe; the sampling bottle is used to collect the liquid phase sample discharged from the drain pipe; the back pressure pump is used to depressurize; and the back pressure replenishment bottle is used to collect excess liquid in the drain pipe.
[0029] The gas phase acquisition system includes a gas sampling bag and a quick interface. The quick interface is connected to the reaction chamber and is used to export gas to the gas sampling bag.
[0030] The monitoring system includes a pressure sensor, a temperature sensor, and a liquid level sensor.
[0031] This application also discloses a continuously sampling dual-compartment reaction method, applied to any of the continuously sampling dual-compartment reaction devices described above, wherein the method includes:
[0032] Step S1: Start the liquid injection system until the liquid completely covers the core to be reacted; start the gas injection system until the preset pressure condition is reached in the reaction chamber.
[0033] Step S2: Control the start of the gas phase acquisition system and the gas injection system, discharge the gas under stable pressure, and seal the reaction chamber after obtaining the target volume of gas phase sample.
[0034] Step S3: Control the start of the liquid phase acquisition system and the liquid injection system, discharge the liquid when the liquid level is higher than the core to be reacted, and seal the reaction chamber after obtaining the target volume of liquid phase sample.
[0035] Step S4: Control the gas injection system to inject gas into the sampling chamber until the pressure conditions of the sampling chamber are the same as those of the reaction chamber; control the gate valve to open and start the core pushing system to push the core into the sampling chamber; after the core has completely entered the sampling chamber, close the gate valve and depressurize until the pressure in the sampling chamber is the same as atmospheric pressure, then open the sampling chamber, remove the core, and complete a single core sampling.
[0036] The continuously sampling dual-chamber reaction method comprises a reaction vessel and a core holder rotatably mounted on the reaction vessel. The reaction vessel contains a reaction chamber, and a gate valve is mounted on the top of the reaction chamber to connect to the sampling chamber. The bottom end of the core holder extends into the reaction chamber and is provided with multiple staggered fixing frames. The fixing frames have multiple ring-shaped locking holes for securing the core sample inserted into the reaction chamber.
[0037] After step S4, the method further includes:
[0038] Step S5: Control the core holder to rotate until another core is aligned with the gate valve; then repeat step S4 to complete continuous core sampling.
[0039] Compared with the prior art, the embodiments of the present invention have the following advantages:
[0040] The dual-chamber reaction device for continuous sampling disclosed in this invention maintains a high-pressure experimental state during sampling, minimizing the impact on the environment within the reaction chamber. Specifically, when removing solid samples, the core is first moved to the sampling chamber, and then the gate valve is closed to isolate the sampling chamber from the reaction chamber. This ensures that depressurization will not affect the experimental state within the reaction chamber. When removing liquid and gaseous samples, the pressure value under experimental conditions can be maintained by simultaneously activating the liquid injection system and the gas injection system. Furthermore, during sampling, data is collected through a monitoring system, and the collected data is processed by the control system to adjust the experimental state within the reaction chamber in real time, thereby maintaining a stable pressure.
[0041] In summary, this invention is based on the design concept of dual-chamber pressure balance and dedicated phase sampling. It sets up a dual-chamber structure consisting of a reaction chamber and a sampling chamber, equipped with a high-pressure sealable gate valve and a dedicated gas, liquid and solid sampling system. It can achieve accurate and efficient sampling of multiphase samples under pressure-free conditions, adapt to the requirements of high-pressure carbon dioxide mineralization reaction experiments, improve sampling reliability and data accuracy, and provide reliable equipment support for carbon dioxide mineralization experimental research. Attached Figure Description
[0042] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0043] Figure 1 This is a simplified structural diagram of the dual-compartment reaction device capable of continuous sampling in this invention;
[0044] Figure 2 This is a schematic diagram of the dual-compartment structure reaction device capable of continuous sampling in this invention.
[0045] Figure 3 This is a schematic diagram of the reactor, sampling chamber, core holder, and core delivery system in the assembled state of the present invention;
[0046] Figure 4 for Figure 3 Cross-sectional view along the AA' direction;
[0047] Figure 5 This is a flowchart of the continuously sampling dual-compartment reaction method in this invention;
[0048] Figure 6 This is a diagram illustrating the experimental steps of the continuously sampled dual-compartment reaction method of the present invention.
[0049] Figure 7 This is a diagram illustrating the application environment of the dual-compartment reaction method based on continuous sampling in this invention.
[0050] Figure 8 This is a schematic diagram of the terminal in this invention.
[0051] Among them, 10 is the reaction chamber; 11 is the constant temperature water bath; 12 is the reaction vessel; 121 is the bottom chamber; 122 is the reaction chamber; 123 is the sampling channel; 124 is the connecting hole; 13 is the core holder; 131 is the rotary valve; 132 is the fixing frame; 1321 is the locking hole; 14 is the first viewing window; 20 is the sampling chamber; 21 is the second viewing window; 30 is the gate valve; 40 is the core pushing system; 41 is the lifting device; 42 is the pushing support; and 50 is the liquid injection system. 51. Liquid injection pump; 52. Liquid storage bottle; 60. Gas injection system; 61. Gas injection pump; 62. Gas cylinder; 70. Liquid phase acquisition system; 71. Drainage pipeline; 72. Back pressure valve; 73. Back pressure pump; 74. Back pressure replenishment bottle; 75. Liquid collection bottle; 80. Gas phase acquisition system; 81. Gas collection bag; 82. Quick interface; 90. Monitoring system; 91. Pressure sensor; 92. Temperature sensor; 100. Control system; 102. Terminal; 104. Server. Detailed Implementation
[0052] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0053] Due to manufacturing techniques and / or tolerances, variations in the shapes shown in the accompanying drawings may occur. Therefore, the examples described herein are not limited to the specific shapes shown in the drawings, but include changes in shape that may occur during manufacturing. The flowcharts shown in the accompanying drawings are merely illustrative and do not necessarily include all contents, operations, or steps, nor do they necessarily need to be performed in the order described. For example, some operations or steps may be broken down, combined, or partially merged, so the actual order of execution may change depending on the specific circumstances.
[0054] As used herein, the term “and / or” includes any one of the relevant items listed and any combination of any two or more items.
[0055] Although terms such as “first,” “second,” and “third” may be used herein to describe individual components, systems, regions, layers, or parts, these components, systems, regions, layers, or parts are not limited by these terms. Rather, these terms are used only to distinguish one component, system, region, layer, or part from another. Therefore, without departing from the teachings of the examples described herein, the first component, system, region, layer, or part referred to as the second component, system, region, layer, or part may also be referred to as the second component, system, region, layer, or part.
[0056] For ease of description, spatial relational terms such as “above,” “upper,” “below,” and “lower” are used herein to describe the relationship between one element and another, as shown in the accompanying drawings. Such spatial relational terms are intended to encompass not only the orientation depicted in the drawings but also different orientations of the device during use or operation. For example, if the device in the drawings is flipped, an element described as being “above” or “upper” relative to another element will subsequently be “below” or “lower” relative to that other element. Therefore, the term “above” includes both “above” and “below” orientations depending on the spatial orientation of the device. The device may also be positioned in other ways, and the spatial relational terms used herein will be interpreted accordingly.
[0057] The terminology used herein is for the purpose of describing various examples only and is not intended to limit this disclosure. Unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. The terms “comprising,” “including,” and “having” enumerate the stated features, quantities, operations, components, elements, and / or combinations thereof, but do not exclude the presence or addition of one or more other features, quantities, operations, components, elements, and / or combinations thereof.
[0058] Carbon dioxide mineralization technology, capable of simultaneously achieving permanent carbon dioxide sequestration and resource utilization, has become a research hotspot in the field of climate change response. In static experimental studies, accurately obtaining liquid, gas, and solid samples within the reaction system is crucial for elucidating reaction mechanisms, analyzing kinetic characteristics, and optimizing process parameters. However, existing static reaction apparatuses have significant shortcomings in their sampling procedures. First, sampling requires depressurization, which instantly disrupts the pressure balance of the reaction system, causing dissolved CO2 to escape, interfering with or even interrupting the mineralization reaction, making the sample unrepresentative of the true state. Furthermore, the depressurization process easily introduces external impurities that contaminate the sample. Repressurization is also necessary after sampling, which is time-consuming and reduces experimental efficiency and data comparability. Second, multiphase sampling has poor compatibility; a single sampling channel easily leads to cross-contamination of gas, liquid, and solid samples, while multiple samplings repeatedly disturb the reaction system. Third, the apparatus lacks sufficient high-pressure sealing performance, making it prone to leakage under the high-pressure conditions required for the mineralization reaction. This not only affects pressure stability and experimental accuracy but also poses safety hazards.
[0059] In summary, the problems of existing devices in the sampling process, such as disrupting reaction equilibrium, easy introduction of contamination, poor compatibility of multiphase sampling, and unreliable high-pressure sealing, have become key bottlenecks restricting in-depth research on carbon dioxide mineralization technology.
[0060] See Figure 1One embodiment of this invention discloses a dual-chamber reaction device capable of continuous sampling, comprising a reaction chamber 10, a sampling chamber 20, a core delivery system 40, a liquid injection system 50, a gas injection system 60, a liquid phase acquisition system 70, a gas phase acquisition system 80, a monitoring system 90, and a control system 100. The sampling chamber 20 is located at the top of the reaction chamber 10; a gate valve 30 is provided between the sampling chamber 20 and the reaction chamber 10; the core delivery system 40 is vertically and vertically mounted within the reaction chamber 10, used to hold the core samples to be reacted and to deliver the core samples to the sampling chamber 20.
[0061] Both the liquid injection system 50 and the gas injection system 60 are connected to the reaction chamber 10; the liquid injection system 50 is used to inject a solution into the reaction chamber 10; the gas injection system 60 is used to inject experimental gas into the reaction chamber 10.
[0062] Specifically, the liquid injection system 50 is connected to the reaction chamber 10 via a connector located on the side wall of the reaction chamber 10, near the bottom, to facilitate liquid injection from a lower position and gradually raise the liquid level. The gas injection system 60 is also connected to the reaction chamber 10 via a connector located on the side wall of the reaction chamber 10, near the top, to facilitate gas injection from a higher position. This distribution method staggers the liquid injection system 50 and the gas injection system 60 vertically, ensuring that gas injection and liquid injection operations do not interfere with each other and can be performed simultaneously, making operation convenient.
[0063] Both the liquid phase acquisition system 70 and the gas phase acquisition system 80 are connected to the reaction chamber 10; the liquid phase acquisition system 70 is used to acquire liquid phase samples; and the gas phase acquisition system 80 is used to acquire gas phase samples.
[0064] Specifically, the liquid phase acquisition system 70 is connected to the side wall of the reaction chamber 10 and is located near the bottom of the reaction chamber 10. It is preferably positioned opposite the connection point of the liquid injection system 50 to achieve the effect of liquid inlet on one side and liquid outlet on the other side without mutual interference. The gas phase acquisition system 80 is connected to the side wall of the reaction chamber 10 and is located near the top of the reaction chamber 10. It is preferably positioned opposite the connection point of the gas injection system 60 to minimize the mutual interference between gas inlet and outlet and improve the accuracy of gas sampling.
[0065] The monitoring system 90 is connected to the reaction chamber 10 and is used to collect the operating parameters inside the reaction chamber 10. The monitoring system 90 can be connected to the top wall or side wall of the reaction chamber 10 as needed. The control system 100 is electrically connected to the core pushing system 40, the liquid injection system 50, the gas injection system 60, the liquid phase acquisition system 70, the gas phase acquisition system 80, and the monitoring system 90, and is used to maintain the pressure value inside the reaction chamber 10.
[0066] The dual-chamber structure reaction device with continuous sampling disclosed in this embodiment can maintain a stable pressure value during sampling, maintain a high-pressure experimental state, and reduce the impact on the environment inside the reaction chamber 10. Specifically, when taking out solid samples, the core is first moved to the sampling chamber 20, and then the gate valve 30 is closed to isolate the sampling chamber 20 from the reaction chamber 10. This way, the experimental state inside the reaction chamber 10 will not be affected when depressurizing. When taking out liquid and gas samples, the pressure value under experimental conditions can be maintained by simultaneously activating the liquid injection system 50 and the gas injection system 60.
[0067] Furthermore, during the sampling process, data is collected through the monitoring system 90, including but not limited to operating parameters such as temperature, pressure, and gas consumption. The collected data is processed by the control system 100, which can adjust the experimental status within the reaction chamber 10 in real time to maintain a stable pressure.
[0068] In summary, based on the dual-chamber pressure balance and dedicated phase sampling design concept, the reaction chamber 10 and sampling chamber 20 are set up to form a dual-chamber structure. Equipped with a high-pressure sealable gate valve 30 and a dedicated gas, liquid and solid sampling system, it can achieve accurate and efficient sampling of multiphase samples under pressure-free conditions. It is suitable for the requirements of high-pressure carbon dioxide mineralization reaction experiments, improves sampling reliability and data accuracy, and provides reliable equipment support for carbon dioxide mineralization experimental research.
[0069] like Figure 2 As shown in another embodiment of this application, the reaction chamber 10 includes a constant temperature water bath 11 and a reaction vessel 12 placed in the constant temperature water bath 11. Placing the reaction vessel 12 in the constant temperature water bath 11 helps maintain the temperature stability of the reaction vessel 12, making the temperature control inside the reaction vessel 12 more accurate and increasing the stability of the experimental environment. Preferably, a transparent constant temperature water bath 11 can be used to facilitate real-time observation of the conditions inside the bath and convenient adjustment of the device at any time.
[0070] like Figure 3 and Figure 4As shown, the reactor 12 disclosed in this embodiment has a bottom chamber 121 and a reaction chamber 122. The liquid injection system 50, the gas injection system 60, the liquid phase acquisition system 70, the gas phase acquisition system 80, and the monitoring system 90 are all connected to the reactor 12 and extend into the reaction chamber 122. A sampling channel 123 communicating with the reaction chamber 122 is provided at the top of the reactor 12, and the sampling channel 123 is used to connect to the sampling chamber 20. A gate valve 30 is provided on the reactor 12 for opening and closing the sampling channel 123.
[0071] In this embodiment, the core sample to be reacted is placed into the sampling chamber 20, then downwards through the sampling channel 123 into the reaction vessel 12. After the core sample is placed, the gate valve 30 is closed, forming a sealed space within the reaction vessel 12. This embodiment utilizes a high-temperature, high-pressure reaction vessel 12, which can create a high-pressure experimental environment by injecting liquids or gases. The experimental status is monitored in real-time by the monitoring system 90. Once the experimental conditions are met, samples are taken under pressure using the liquid phase acquisition system 70 and the gas phase acquisition system 80 to obtain liquid and gas phase samples. Simultaneously, during the experiment, the core sample can be moved upwards into the sampling chamber 20. As long as the pressure conditions of the sampling chamber 20 and the reaction chamber 10 are kept consistent, pressure-holding sampling can be achieved, thus achieving continuous multiphase sampling of gas, liquid, and solid phases.
[0072] The core delivery system 40 disclosed in this embodiment is located in the bottom chamber 121, below the reaction chamber 122. A connecting hole 124 is provided at the bottom of the reaction chamber 122, directly opposite the sampling channel 123. The core delivery system 40 passes through the connecting hole 124 and is inserted into the reaction chamber 122 to hold the core to be reacted and to deliver the core to the sampling chamber 20.
[0073] In this embodiment, the core is moved by a core pushing system 40, which is located in the bottom chamber 121. This system isolates the high-pressure environment within the reaction chamber 122, prevents liquid contamination, reduces corrosion, and extends the service life. The core pushing system 40 is adapted to the connecting hole 124, allowing it to extend upwards to push the core.
[0074] For example Figure 3 and Figure 4As shown, in another embodiment of this application, the reaction chamber 10 further includes a core holder 13, which extends longitudinally and is rotatably mounted on the reaction vessel 12. A rotary valve 131 is provided at the top of the core holder 13, which is used to drive the core holder 13 to rotate. The bottom end of the core holder 13 extends into the reaction chamber 122 and is provided with multiple layers of staggered fixing frames 132. The fixing frames 132 are provided with a plurality of ring-shaped locking holes 1321, the diameter of which is equal to the diameter of the sampling channel 123, so as to constrain the core to be reacted inserted into the reaction chamber 122.
[0075] In this embodiment, the core sample to be reacted is placed inside the reaction chamber 122 and held upright by the core retainer 13 to prevent it from tipping over and colliding with the inner wall of the reactor 12. Specifically, the core retainer 13 is equipped with multi-layered fixing frames 132 of different heights, and each fixing frame 132 is provided with a locking hole 1321, so that the core sample can be supported from different heights, further improving the stability of the core sample.
[0076] In this embodiment, the diameter of the locating hole 1321 is matched with the diameter of the sampling channel 123 to adapt to the size of the core, so that the sidewall of the locating hole 1321 fits as closely as possible to the outer sidewall of the core. In other words, improving the fit between the locating hole 1321 and the core reduces core movement and collisions between the core and the core holder 132. Moreover, accurate positioning allows the core holder 13 to move the core.
[0077] Specifically, in this embodiment, multiple core samples can be placed in the reaction chamber 122 to improve experimental efficiency. In this case, the rotary valve 131 can rotate the core holder 13, moving the core sample placed in the reaction chamber 122 to another position in the reaction chamber 122, making the position opposite the sampling channel 123 empty, so that subsequent core samples can be placed in again.
[0078] Similarly, during the sampling process, after one core from the reaction chamber 122 is pushed into the sampling chamber 20, another core can be moved to the position aligned with the sampling channel 123 by rotating the core holder 13, and the core pushing system 40 is restarted to send out the core again.
[0079] In summary, by setting up a rotatable core holder 13, multiple cores can be placed or removed in an orderly manner, increasing the orderliness of the experiment and improving experimental efficiency.
[0080] For example Figure 4As shown, the reactor 12 disclosed in this embodiment has an opening at its center, allowing the core holder 132 to be inserted into the center of the reactor 12. When the core holder 132 rotates, the probability of it colliding with the reactor 12 is reduced. Furthermore, the sampling channel 123 disclosed in this embodiment surrounds the core holder 132, so that the locking holes 1321 on the core holder 132 are aligned with the sampling channel 123, facilitating the placement and removal of the core.
[0081] In addition, during the experiment, the gas is introduced into the reaction chamber 10 and dissolves into the liquid, which takes a certain amount of time. The rotatable core holder 13 can be set up to act as a stirrer. Stirring the solution can accelerate the dissolution rate of the gas and reduce the solution saturation time.
[0082] Specifically, as another embodiment of this application, it is disclosed that multiple sampling channels 123 are provided, and the multiple sampling channels 123 are arranged in a ring along the circumference of the reactor 12; multiple gate valves 30 are provided, and one gate valve 30 is provided at each sampling channel 123; multiple sampling chambers 20 are provided, and each sampling channel 123 is connected to one sampling chamber 20.
[0083] In this embodiment, the multiple sampling channels 123 can be used to insert different core samples to be reacted, thereby improving the efficiency of a single experiment. During sample placement, each sampling chamber 20 and each gate valve 30 can be opened separately. After all core samples are placed, all sampling chambers 20 are closed, and all gate valves 30 are shut off. During sampling, the corresponding gate valve 30 and the corresponding sampling chamber 20 are opened sequentially, allowing multiple core samples to be retrieved in stages. While maintaining stable high pressure in the device, multiple solid-phase samples can be obtained continuously, improving experimental efficiency and enhancing sampling reliability and data accuracy.
[0084] For example Figure 3 and Figure 4 As shown, in another embodiment of this invention, three sampling channels 123 are provided on the top of the reactor 12. The diameter of the sampling channels 123 is 30 mm. The sampling chamber 20 is a small visual vessel. All three small visual vessels are connected to the reactor 12, and three gate valves 30 are provided to match the three small visual vessels. During the experiment, by pressurizing the small visual vessels and the reactor 12 respectively, the pressure environment of the two can be balanced, and solid core sampling can be achieved under non-depressurization conditions.
[0085] Specifically, the sampling chamber 20 disclosed in this embodiment is openable, and a corrosion-resistant rubber ring can be installed at the opening of the sampling chamber 20 to maintain its sealing performance for a long time. After the core is moved into the sampling chamber 20, the sampling chamber 20 is depressurized separately, and then the core can be safely removed.
[0086] like Figure 4As shown, in another embodiment of this application, the core pushing system 40 is disclosed, including a lifter 41 and a pusher support 42. The lifter 41 is disposed in the bottom chamber 121, and the movable end of the lifter 41 can move toward the connecting hole 124. The pusher support 42 is disposed at the movable end of the lifter 41. The diameter of the pusher support 42 is equal to the diameter of the connecting hole 124.
[0087] The lifting device 41 disclosed in this embodiment includes, but is not limited to, hydraulic rods, gear transmission rods, spring rods, etc., or it can also be a magnetic rod, driven by a magnetic attraction generator (e.g., an electromagnet) installed outside the reaction vessel 12. The lifting device 41 is arranged longitudinally and can move back and forth in the vertical direction. The top of the lifting device 41 is provided with the pusher support 42, which can be connected by welding, snap-fit, or other methods to form a whole, making the structure of the core pushing system 40 stable. When the lifting device 41 is raised, it lifts the pusher support 42 from the connecting hole 124 into the reaction chamber 122, thereby driving the pusher support 42 to rise and fall, realizing the function of pushing the core.
[0088] Specifically, the diameter of the pusher 42 is equal to the diameter of the connecting hole 124, so the pusher 42 and the connecting hole 124 are in a tight fit. During the process of the pusher 42 rising, at least a part of the bottom is retained in the connecting hole 124 to maintain the separation between the reaction chamber 122 and the bottom chamber 121, which can prevent the reaction chamber 122 from leaking air or liquid and maintain the high pressure and stable pressure state in the reaction chamber 122.
[0089] like Figure 3 and Figure 4 As shown in another embodiment of this application, the reaction chamber 10 is provided with a first viewing window 14; the sampling chamber 20 is provided with a second viewing window 21. Both the first viewing window 14 and the second viewing window 21 disclosed in this embodiment can be made of high-strength glass to maintain the integrity of the reaction chamber 10 and the sampling chamber 20. Simultaneously, the environmental conditions inside the reaction chamber 10 or the sampling chamber 20 can be directly obtained through visual observation, facilitating rapid assessment of the core sample's condition, better control of the experimental process, and improved experimental safety.
[0090] like Figure 2As shown in another embodiment of this application, the injection system 50 includes an injection pump 51 and a storage bottle 52. The storage bottle 52 is used to store the experimental solution. One end of the injection pump 51 is connected to the storage bottle 52, and the other end is connected to the reaction chamber 10, for injecting the solution into the reaction chamber 10. The injection pump 51 disclosed in this embodiment includes, but is not limited to, centrifugal pumps, reciprocating pumps, peristaltic pumps, etc. The storage bottle 52 stores a pre-prepared solution. When the liquid level in the reaction chamber 10 drops and is insufficient to submerge the core, the injection pump 51 can be activated to replenish the liquid, thereby maintaining the stability of the experimental state.
[0091] For example Figure 2 As shown, in another embodiment of this application, the gas injection system 60 is disclosed to include a gas injection pump 61 and a gas cylinder 62, the gas cylinder 62 being used to store carbon dioxide gas; one end of the gas injection pump 61 is connected to the gas cylinder 62, and the other end is connected to the reaction chamber 10, for injecting carbon dioxide gas into the reaction chamber 10.
[0092] The gas injection pump 61 disclosed in this embodiment includes, but is not limited to, a pneumatic diaphragm pump. By continuously replenishing the reaction chamber 10 with gas via the gas injection pump 61, the high-pressure state within the reaction chamber 10 can be maintained, further improving the stability of the experimental state.
[0093] For example Figure 2 As shown, in another embodiment of this application, the liquid phase acquisition system 70 includes a drain pipe 71 connected to the reaction chamber 10, a back pressure valve 72, a back pressure pump 73, and a back pressure replenishment bottle 74 sequentially arranged on the drain pipe 71, and a sampling bottle 75 connected to the back pressure valve 72; the back pressure valve 72 is used to open or close the drain pipe 71; the sampling bottle 75 is used to collect the liquid phase sample discharged from the drain pipe 71, the back pressure pump 73 is used to depressurize; and the back pressure replenishment bottle 74 is used to collect excess liquid in the drain pipe 71.
[0094] The liquid phase acquisition system 70 disclosed in this embodiment is used to extract liquid phase samples under stable pressure. Therefore, during sampling, the back pressure valve 72 is first opened to export the liquid phase sample to the sampling bottle 75, and then the back pressure valve 72 is closed to isolate the reaction chamber 10 and avoid affecting the experimental environment within the reaction chamber 10. At this time, the liquid in the sampling bottle 75 is still under high pressure, so the back pressure pump 73 can be activated to release the pressure, making the pressure environment inside the sampling bottle 75 equal to atmospheric pressure, and excess liquid is collected through the back pressure replenishment bottle 74. After completing the above operations, the liquid phase sample in the sampling bottle 75 can be collected, ending the sampling operation.
[0095] As can be seen, the liquid phase acquisition system 70 disclosed in this embodiment can acquire liquid phase samples in an orderly, efficient and safe manner without affecting the pressure environment of the reaction chamber 10, thereby improving the safety of the experiment, enhancing the effectiveness of the experimental samples, and increasing the reliability of the experimental results.
[0096] For example Figure 2 As shown in another embodiment of this application, the gas phase acquisition system 80 includes a gas collection bag 81 and a quick-connect interface 82. The quick-connect interface 82 is connected to the reaction chamber 10 and is used to export gas to the gas collection bag 81. The quick-connect interface 82 disclosed in this embodiment can be a quick-release switch connector, with the inlet inserted into the reaction chamber 10 and the outlet connected to the gas collection bag 81. During sampling, by opening the quick-connect interface 82, the gas in the reaction chamber 10 slowly and evenly flows out into the gas collection bag 81, thus collecting the gas phase sample. This collection method eliminates the need to depressurize the entire reaction chamber 10, resulting in high collection efficiency and reducing the problem of cross-contamination in multiphase sampling.
[0097] For example Figure 2 As shown in another embodiment of this application, the monitoring system 90 includes a pressure sensor 91, a temperature sensor 92, and a liquid level sensor. In the reaction chamber 10 disclosed in this embodiment, it is primarily necessary to maintain stable temperature and pressure conditions. Therefore, the temperature sensor 92 and the pressure sensor 91 are installed to facilitate the timely acquisition of real-time temperature and pressure data. These data are then adjusted by the control system 100 at any time, thereby increasing the response speed and maintaining a high-pressure state within the reaction chamber 10 during continuous sampling or multiphase sampling, further improving sampling reliability and data accuracy.
[0098] like Figure 5 As shown, as another embodiment of this application, a continuously sampling dual-compartment reaction method is also disclosed, applied to any of the continuously sampling dual-compartment reaction devices described above, wherein the method includes:
[0099] Step S1: Start the liquid injection system 50 until the liquid completely covers the core to be reacted; start the gas injection system 60 until the preset pressure condition is reached in the reaction chamber 10.
[0100] In this embodiment, the sampling chamber 20 is opened beforehand, and the core sample to be reacted is placed inside, extending into the reaction chamber 10 through the gate valve 30. Then, the sampling chamber 20 and the gate valve 30 are closed, allowing the core sample to be tested in a closed environment within the reaction chamber 10. With the reaction chamber 10 completely sealed, liquid and gas are injected to completely submerge the core sample, with the liquid level above the top surface of the core sample. The introduced gas dissolves in the liquid, forming a saturated solution. Furthermore, the pressure is continuously increased during the continuous gas injection process until a preset pressure condition (generally higher than atmospheric pressure) is reached, completing the dissolution equilibrium.
[0101] Step S2: Control the start of the gas phase acquisition system 80 and the gas injection system 60, discharge the gas under stable pressure, and after obtaining the target volume of gas phase sample, seal the reaction chamber 10.
[0102] Step S3: Control the start of the liquid phase acquisition system 70 and the liquid injection system 50, discharge the liquid when the liquid level is higher than the core to be reacted, and after obtaining the target volume of liquid phase sample, seal the reaction chamber 10.
[0103] Step S4: Control the gas injection system 60 to inject gas into the sampling chamber 20 until the pressure conditions of the sampling chamber 20 are the same as those of the reaction chamber 10; control the gate valve 30 to open and start the core pushing system 40 to push the core into the sampling chamber 20; after the core has completely entered the sampling chamber 20, control the gate valve 30 to close and depressurize until the pressure inside the sampling chamber 20 is the same as atmospheric pressure, then open the sampling chamber 20, remove the core, and complete a single core sampling.
[0104] The reaction method disclosed in this embodiment takes into account the sampling requirements of gas phase, liquid phase and solid phase, avoids the disturbance of the reaction system by depressurization, solves the problem of cross-contamination in multiphase sampling, adapts to the experimental requirements of high-pressure carbon dioxide mineralization reaction, improves sampling reliability and data accuracy, and provides equipment support for the study of carbon dioxide mineralization mechanism.
[0105] It should be noted that steps S2 to S4 disclosed in this embodiment are for sampling different types of samples, and the order is not important; the sequence can be adjusted according to actual operational requirements. The common effect of steps S2 to S4 is that, regardless of what sample is taken out, the pressure value inside the reaction chamber 10 can be kept stable, thereby avoiding affecting the experimental environment, keeping the experimental process continuous, and facilitating continuous sampling.
[0106] Specifically, as another embodiment of this application, the reaction chamber 10 is also disclosed to include a reaction vessel 12 and a core holder 13 rotatably mounted on the reaction vessel 12. The reaction vessel 12 is provided with a reaction chamber 122, and the top of the reaction chamber 122 is provided with the gate valve 30 to connect to the sampling chamber 20. The bottom end of the core holder 13 extends into the reaction chamber 122 and is provided with multiple layers of staggered fixing frames 132. The fixing frames 132 are provided with a plurality of ring-shaped locking holes 1321, which are used to restrain the core to be reacted inserted into the reaction chamber 122.
[0107] After step S4, the method further includes:
[0108] Step S5: Control the core holder 13 to rotate until another core is aligned with the gate valve 30; then repeat step S4 to complete continuous core sampling.
[0109] As can be seen, by continuous sampling, solid-phase samples with different reaction times can be obtained, thereby increasing the dimensions of comparative analysis and enabling more in-depth research and analysis.
[0110] Specifically, such as Figure 6 As shown, another embodiment of this invention discloses the following steps for a continuously sampling dual-compartment reaction method:
[0111] I. Experimental Preparation
[0112] 1. Determine the required temperature and pressure conditions for the experiment, check the sealing of the apparatus, and correctly connect the gas inlet, liquid inlet, and liquid outlet.
[0113] 2. Prepare core samples according to the test conditions. The core sample diameter should be less than 30 mm and the height should be less than 60 mm.
[0114] 3. Place the core samples to be reacted into the core holder 13 inside the reaction chamber 10 through the three sampling channels 123 reserved above the chamber. The core holder 13 has six staggered locking holes 1321, and each layer of the holder 132 has three locking holes 1321 spaced 120° apart. Adjacent layers of holders 132 are staggered, allowing a total of six core samples to be placed. First, place three core samples in the initial position. Then, rotate the rotary valve 131 of the core holder 13 by a certain angle to place the remaining three. Finally, close the gate valve 30 and the drain valve to ensure the reaction chamber 10 is sealed.
[0115] II. Dissolution Equilibrium
[0116] 1. Inject a solution into the reaction chamber 10 using the injection pump 51. In this embodiment, the solution can be formation water or other solutions selected according to experimental requirements. Observe the liquid level in the reaction chamber 10 through the visualization window. Stop the injection when the liquid level is higher than the core.
[0117] 2. Gas, such as CO2, is injected into the reaction chamber 10 via the gas injection pump 61. During the injection process, the pressure inside the reaction chamber 10 gradually increases. The pressure data is collected in real time by the pressure sensor 91 and sent to the control system 100. The control system 100 stabilizes the gas pressure at the pressure conditions required for the reaction. During this period, CO2 gradually dissolves in the solution. Once the solution reaches saturation, the gas injection can be stopped.
[0118] III. Gas Sampling
[0119] The gas sampling bag 81 is fixed to the quick-connect interface 82 with a valve. The quick-connect interface 82 is connected to the exhaust port of the reactor 12. The valve on the quick-connect interface 82 is slightly opened to allow the gas to be discharged into the gas sampling bag 81 at a very slow speed. At the same time, the pressure sensor 91 collects pressure data in the reaction chamber 10. When the pressure drops, the control system 100 promptly controls the gas injection system 60 to start, so as to automatically track and adjust the pressure to maintain the pressure required for the reaction in the reaction chamber 10. After the gas is collected, the valve on the quick-connect interface 82 is closed, thus completing the gas sampling without pressure relief.
[0120] IV. Liquid Sampling
[0121] 1. The back pressure pump 73 is set to a pressure 1-2 MPa lower than the required reaction pressure. The control system 100 automatically tracks and adjusts the pressure in the reaction chamber 10 to maintain it at a pressure 1-2 MPa higher than the required reaction pressure. Simultaneously, a liquid level sensor is installed in the reaction chamber 10. When the liquid level falls below a specific value, the control system 100 automatically activates the injection pump 51 to replenish the liquid in the reaction vessel 12.
[0122] 2. When a pressure difference is generated, the liquid in the reaction chamber 10 is discharged through the drain outlet on the reaction vessel 12 and enters the sampling bottle 75. The sampling bottle 75 is equipped with a quick interface 82 and is marked with a volume scale. When the liquid reaches the required volume, the drain outlet is closed and the pressure is released by the back pressure pump 73. Finally, the sampling bottle 75 is taken out, and the liquid sampling without pressure release is completed.
[0123] V. Pressure Balance Regulation
[0124] The sampling chamber 20 is fixed above the sampling channel 123 reserved in the reaction chamber 10. One sampling chamber 20 or three sampling chambers 20 can be used together.
[0125] 1. First, close the exhaust valve of sampling chamber 20 to ensure that sampling chamber 20 is sealed.
[0126] 2. Inject CO2 gas into the sampling chamber 20 through the gas injection valve above the sampling chamber 20. During the injection process, the pressure inside the chamber will gradually increase until the gas pressure stabilizes at the pressure conditions required for the reaction. At this time, the pressure of the reaction chamber 10 and the sampling chamber 20 is the same, and the pressure difference between the two sides is zero. Open the gate valve 30 to connect the sampling chamber 20 and the reaction chamber 10.
[0127] VI. Solid Sampling
[0128] 1. After the pressure balance is adjusted, the control system 100 issues a control command, which can control one or all three lifters 41 simultaneously, causing the pusher 42 to push the core upward at a speed of 5 mm / s. The core is constrained by the core holder 13 and moves vertically upward, passing through the sampling channel 123 at the top of the reaction chamber 10. When it passes through the gate valve 30, the gate valve 30 is closed, and the pusher 42 is lowered to its initial position via the connected lifter 41. The reaction chamber 10 can remain closed for subsequent reactions.
[0129] 2. Once the core sample is inside the sampling chamber 20, open the exhaust valve of the sampling chamber 20 to reduce the internal pressure of the sampling chamber 20 by venting until the internal pressure is the same as atmospheric pressure. Finally, open the sampling chamber 20 and take out the core sample, thus completing the unrelieved solid sampling.
[0130] As can be seen, the dual-chamber structure reaction device and method of the present invention can be directly observed to push the core from the reaction chamber 10 to the sampling chamber 20, ensuring that the core is sampled without deflection or pressure impact, thus ensuring the integrity of the core sample and the continuity and accuracy of the experimental data.
[0131] The continuously sampling dual-compartment reaction method provided in this invention can be applied to, for example... Figure 7 In the application environment shown, terminal 102 communicates with server 104 via a network. A data storage system can store the data that server 104 needs to process. The data storage system can be integrated onto server 104, or it can be located in the cloud or on another network server. The continuously sampling dual-compartment reaction method can be executed by terminal 102 or server 104, or it can be executed collaboratively by terminal 102 and server 104. Of course, the continuously sampling dual-compartment reaction method of this embodiment can also be implemented based on the control system 100 of the continuously sampling dual-compartment reaction equipment itself.
[0132] Specifically, the control system 100 disclosed in this embodiment can be a smartphone, tablet computer, laptop computer, desktop computer, smart speaker, smartwatch, etc. The server 104 can be an independent physical server or a service node in a blockchain system, in which the service nodes form a peer-to-peer network.
[0133] In addition, server 104 can also be a server cluster consisting of multiple physical servers, which can be a cloud server that provides basic cloud computing services such as cloud services, cloud databases, cloud computing, cloud functions, cloud storage, network services, cloud communication, middleware services, domain name services, security services, content delivery networks (CDN), and big data and artificial intelligence platforms.
[0134] Terminal 102 and server 104 can be connected via Bluetooth, USB (Universal Serial Bus) or network communication, and the present invention does not limit this connection.
[0135] In some embodiments, a terminal is provided, the internal structure of which can be as follows: Figure 8 As shown, the terminal includes a processor, memory, input / output interface, communication interface, display unit, and input device. The processor, memory, and input / output interface are connected via a system bus, and the communication interface, display unit, and input device are also connected to the system bus via the input / output interface. The processor provides computing and control capabilities. The memory includes non-volatile storage media and internal memory. The non-volatile storage media stores the operating system and computer programs. The internal memory provides the environment for the operation of the operating system and computer programs stored in the non-volatile storage media. The input / output interface is used for exchanging information between the processor and external devices. The communication interface is used for wired or wireless communication with external terminals; wireless communication can be achieved through Wi-Fi, mobile cellular networks, NFC (Near Field Communication), or other technologies.
[0136] When executed by a processor, the computer program implements a continuously sampled dual-compartment reaction method. The terminal's display unit is used to form a visually visible image and can be a display screen, a projection device, or a virtual reality imaging device. The display screen can be an LCD screen or an e-ink screen. The terminal's input device can be a touch layer covering the display screen, buttons, a trackball, or a touchpad on the terminal casing, or an external keyboard, touchpad, or mouse.
[0137] Those skilled in the art will understand that Figure 8 The structure shown is merely a block diagram of a portion of the structure related to the present invention and does not constitute a limitation on the terminal to which the present invention is applied. A specific terminal may include more or fewer components than those shown in the figure, or combine certain components, or have different component arrangements.
[0138] Those skilled in the art will understand that all or part of the processes in the above embodiments can be implemented by a computer program instructing related hardware. The computer program can be stored in a non-volatile computer-readable storage medium. When the computer program is executed, it can include the processes of the embodiments of the above methods.
[0139] It should be understood that various parts of this application can be implemented using hardware, software, firmware, or a combination thereof. In the above embodiments, multiple steps or methods can be implemented using software or firmware stored in memory and executed by a suitable instruction execution system. If implemented in hardware, as in another embodiment, it can be implemented using any one or a combination of the following techniques known in the art: discrete logic circuits having logic gates for implementing logical functions on data signals, application-specific integrated circuits (ASICs) having suitable combinational logic gates, programmable gate arrays (FPGAs), field-programmable gate arrays (FPGAs), etc.
[0140] Furthermore, the functional units in the various embodiments of this application can be integrated into a processing module, or each unit can exist physically separately, or two or more units can be integrated into a module. The integrated module can be implemented in hardware or as a software functional module. If the integrated module is implemented as a software functional module and sold or used as an independent product, it can also be stored in a computer-readable storage medium.
[0141] In summary, this application discloses a continuously sampling dual-chamber reaction device, comprising a reaction chamber 10, a sampling chamber 20, a core delivery system 40, a liquid injection system 50, a gas injection system 60, a liquid phase acquisition system 70, a gas phase acquisition system 80, a monitoring system 90, and a control system 100. The sampling chamber 20 is located at the top of the reaction chamber 10. A gate valve 30 is provided between the sampling chamber 20 and the reaction chamber 10. The core delivery system 40 is vertically and vertically mounted inside the reaction chamber 10, used to hold the core to be reacted and to deliver the core to the sampling chamber 20. The liquid injection system 50 and the gas injection system 60 are both connected to the reaction chamber 10. The liquid injection system 50 is used to inject liquid into the core. A solution is injected into the reaction chamber 10; the gas injection system 60 is used to inject experimental gas into the reaction chamber 10; the liquid phase acquisition system 70 and the gas phase acquisition system 80 are both connected to the reaction chamber 10; the liquid phase acquisition system 70 is used to collect liquid phase samples; the gas phase acquisition system 80 is used to collect gas phase samples; the monitoring system 90 is connected to the reaction chamber 10 and is used to collect the operating parameters inside the reaction chamber 10; the control system 100 is electrically connected to the core pushing system 40, the liquid injection system 50, the gas injection system 60, the liquid phase acquisition system 70, the gas phase acquisition system 80, and the monitoring system 90, and is used to maintain the pressure value inside the reaction chamber 10.
[0142] Based on the dual-chamber pressure balance and dedicated phase sampling design concept, the reaction chamber 10 and sampling chamber 20 are set up to form a dual-chamber structure. It is equipped with a gate valve 30 that can be sealed under high pressure and a dedicated gas, liquid and solid sampling system, which can realize accurate and efficient sampling of multiphase samples under pressure relief. It is suitable for the requirements of carbon dioxide high pressure mineralization reaction experiments, improves sampling reliability and data accuracy, and provides reliable equipment support for carbon dioxide mineralization experimental research.
[0143] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other.
[0144] It should be noted that this invention uses a continuously sampling dual-compartment structure reaction device and method as an example to introduce the specific structure and working principle of the invention. However, the application of this invention is not limited to the continuously sampling dual-compartment structure reaction device and method, and can also be applied to the production and use of other similar workpieces.
[0145] It should be understood that the present invention is not limited to the precise structure described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope. The scope of the invention is limited only by the appended claims.
[0146] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A dual-compartment reaction device capable of continuous sampling, characterized in that, include: Reaction chamber; A sampling chamber is located at the top of the reaction chamber; a gate valve is installed between the sampling chamber and the reaction chamber; The core delivery system is vertically mounted inside the reaction chamber and is used to hold the core to be reacted and to deliver the core to the sampling chamber. Both the liquid injection system and the gas injection system are connected to the reaction chamber; the liquid injection system is used to inject a solution into the reaction chamber; the gas injection system is used to inject experimental gas into the reaction chamber. Both the liquid phase acquisition system and the gas phase acquisition system are connected to the reaction chamber; the liquid phase acquisition system is used to acquire liquid phase samples; the gas phase acquisition system is used to acquire gas phase samples. A monitoring system, connected to the reaction chamber, is used to collect operating parameters within the reaction chamber; The control system is electrically connected to the core delivery system, the liquid injection system, the gas injection system, the liquid phase acquisition system, the gas phase acquisition system, and the monitoring system, and is used to maintain the pressure value inside the reaction chamber. The reaction chamber includes a constant-temperature water bath and a reaction vessel placed in the constant-temperature water bath. The reaction vessel contains a bottom chamber and a reaction chamber. The liquid injection system, gas injection system, liquid phase acquisition system, gas phase acquisition system, and monitoring system are all connected to the reaction vessel and extend into the reaction chamber. A sampling channel communicating with the reaction chamber is provided at the top of the reaction vessel, and the sampling channel is used to connect to the sampling chamber. A gate valve is provided on the reaction vessel for opening and closing the sampling channel. The core pushing system is located in the bottom chamber, below the reaction chamber. The bottom of the reaction chamber is provided with a connecting hole, which is directly opposite the sampling channel; the core pushing system passes through the connecting hole and is inserted into the reaction chamber to hold the core to be reacted and push the core to the sampling chamber.
2. The continuously sampling dual-compartment reaction device according to claim 1, characterized in that, The reaction chamber also includes a core holder, which extends longitudinally and is rotatably mounted on the reaction vessel; The core holder is equipped with a rotary valve at its top, which is used to drive the core holder to rotate. The bottom end of the core holder extends into the reaction chamber and is provided with multiple layers of staggered fixing frames; the fixing frames are provided with multiple ring-shaped locking holes, the diameter of which is equal to the diameter of the sampling channel, so as to constrain the core to be reacted inserted into the reaction chamber.
3. The continuously sampling dual-compartment reaction device according to claim 1, characterized in that, The sampling channel is provided in multiple ways, and the multiple sampling channels are arranged in a ring around the circumference of the reactor. Multiple gate valves are provided, and one gate valve is provided at each of the sampling channels; The sampling chambers are provided in multiple ways, and each sampling channel is connected to one of the sampling chambers.
4. The continuously sampling dual-compartment reaction device according to claim 1, characterized in that, The core pushing system includes a lifter and a pushing support. The lifter is located in the bottom cavity, and the movable end of the lifter can move toward the connecting hole. The pushing support is located at the movable end of the lifter. The diameter of the pusher support is equal to the diameter of the connecting hole.
5. The continuously sampling dual-compartment reaction device according to any one of claims 1 to 4, characterized in that, The reaction chamber is provided with a first viewing window; the sampling chamber is provided with a second viewing window.
6. The continuously sampling dual-compartment reaction device according to claim 1, characterized in that, The liquid injection system includes a liquid injection pump and a storage bottle, the storage bottle being used to store the experimental solution; one end of the liquid injection pump is connected to the storage bottle, and the other end is connected to the reaction chamber, for injecting the solution into the reaction chamber; The gas injection system includes a gas injection pump and a gas cylinder, the gas cylinder being used to store carbon dioxide gas; one end of the gas injection pump is connected to the gas cylinder, and the other end is connected to the reaction chamber, for injecting carbon dioxide gas into the reaction chamber.
7. The continuously sampling dual-compartment reaction device according to claim 1, characterized in that, The liquid phase acquisition system includes a drain pipe connected to the reaction chamber, a back pressure valve, a back pressure pump, and a back pressure replenishment bottle sequentially arranged on the drain pipe, and a sampling bottle connected to the back pressure valve; the back pressure valve is used to open or close the drain pipe; the sampling bottle is used to collect the liquid phase sample discharged from the drain pipe; the back pressure pump is used to release pressure; and the back pressure replenishment bottle is used to collect excess liquid in the drain pipe. The gas phase acquisition system includes a gas sampling bag and a quick interface. The quick interface is connected to the reaction chamber and is used to export gas to the gas sampling bag. The monitoring system includes a pressure sensor, a temperature sensor, and a liquid level sensor.
8. A continuously sampling dual-compartment reaction method, applied to the continuously sampling dual-compartment reaction apparatus as described in any one of claims 1 to 7, characterized in that, include: Step S1: Start the liquid injection system until the liquid completely covers the core to be reacted; start the gas injection system until the preset pressure condition is reached in the reaction chamber. Step S2: Control the start of the gas phase acquisition system and the gas injection system, discharge the gas under stable pressure, and seal the reaction chamber after obtaining the target volume of gas phase sample. Step S3: Control the start of the liquid phase acquisition system and the liquid injection system, and discharge the liquid while keeping the liquid level higher than the core to be reacted. After obtaining the target volume of liquid phase sample, close the reaction chamber. Step S4: Control the gas injection system to inject gas into the sampling chamber until the pressure conditions of the sampling chamber are the same as those of the reaction chamber; control the gate valve to open and start the core pushing system to push the core into the sampling chamber; after the core has completely entered the sampling chamber, control the gate valve to close and depressurize until the pressure in the sampling chamber is the same as atmospheric pressure, then open the sampling chamber, remove the core, and complete a single core sampling.
9. The continuously sampling dual-compartment reaction method according to claim 8, characterized in that, The reaction chamber includes a reaction vessel and a core holder rotatably mounted on the reaction vessel. The reaction vessel contains a reaction chamber, and the top of the reaction chamber is equipped with the gate valve for connecting to the sampling chamber. The bottom end of the core holder extends into the reaction chamber and is provided with multiple layers of staggered fixing frames. The fixing frames are provided with multiple ring-shaped locking holes for restraining the core to be reacted inserted into the reaction chamber. After step S4, the method further includes: Step S5: Control the core holder to rotate until another core is aligned with the gate valve; Repeat step S4 to complete continuous core sampling.