A dynamic tracking adsorption testing device and method adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in various scenarios

Abstract

This invention relates to a dynamic tracking adsorption testing device and method adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in various scenarios. It addresses the current limitations of devices that cannot dynamically track the adsorption process and lack standardized processing devices and methods for multi-parameter linkage analysis. The dynamic tracking adsorption testing device includes a total reaction control unit, a self-regulating gas supply system, and a gas analysis system. The inlet of the total reaction control unit is connected to the self-regulating gas supply system, and the outlet of the total reaction control unit is connected to the gas analysis system. The dynamic tracking adsorption testing method involves pre-treating the test sample under vacuum activation, followed by adsorption and desorption. Data on the mass change and inlet / outlet concentrations during the adsorption phase are obtained. A triple adsorption capacity calculation model is established based on this data, and the adsorption cycle stability test is performed using the triple adsorption capacity calculation model after data analysis.

Description

Technical Field

[0001] Specifically, this invention relates to a dynamic tracking adsorption testing device and method that adapts to the adsorption performance of adsorbents with different carbon dioxide partial pressures in various scenarios. Background Technology

[0002] With the rapid development of materials science, porous carbon capture materials have become one of the most popular materials, and the demand for testing their adsorption functions is increasing, with devices and technologies gradually maturing. However, some shortcomings still exist. For example, insufficient material pretreatment: most devices cannot achieve vacuum high-temperature activation; limited detection dimensions: relying on a single gas concentration sensor makes it difficult to determine the adsorption saturation point; and limited applicability: traditional reactors are sensitive to sample morphology and are incompatible with bulk or non-homogeneous materials. The incompatibility of reactors with bulk or non-homogeneous materials is mainly based on the reactor's design principles, operating conditions, and the characteristics of the bulk or non-homogeneous materials themselves. The main reason is that in homogeneous reactions, reactants are in the same phase, and there is no issue of phase contact. In heterogeneous reactions, reactants are in different phases, requiring consideration of the contact area and efficiency between phases. Homogeneous reactors do not need to consider phase contact issues, making their design relatively simple. Heterogeneous reactors must consider good phase contact, and their design is usually more complex, such as gas-liquid reactors which need to address the mixing and heat transfer issues between the gas and liquid phases.

[0003] Bulk materials, with their large size and fixed shape, limit their flowability and mixing in reactors. Internal heat and mass transfer barriers may exist within bulk materials, leading to reduced reaction efficiency. Within the reactor, bulk materials may form "hot spots" or "cold spots," affecting the uniformity and stability of the reaction. Furthermore, bulk materials may clog reactor pipes or stirring devices, causing operational difficulties. During prolonged reactions, bulk materials may abrade and fragment, affecting normal reactor operation. Non-homogeneous materials exhibit spatial differences in composition and properties, potentially leading to inhomogeneity and instability in the reaction process. Due to these differences, reaction rates and selectivity may vary at different locations, affecting product quality. The reaction process with non-homogeneous materials is difficult to predict and control accurately, increasing production uncertainty and risk. In summary, reactors are incompatible with bulk or non-homogeneous materials primarily due to limitations imposed by these materials in reactor design principles, operating conditions, and the inherent properties of the materials themselves. To ensure the normal operation of the reactor and the stability of product quality, homogeneous materials are typically used, or special mixing and heat transfer measures are adopted in heterogeneous reactions. Furthermore, the lack of a tail gas analysis module prevents the realization of closed-loop data throughout the entire process. In summary, there is no complete method for detecting the adsorption capacity and cycle stability of gases such as carbon dioxide under wide temperature range conditions. Current devices cannot dynamically track the adsorption process, and there is a lack of standardized processing devices and methods for multi-parameter linkage analysis. Summary of the Invention

[0004] To address the aforementioned challenges, this invention provides a dynamic tracking adsorption testing device and method that adapts to the adsorption performance of adsorbents with different carbon dioxide partial pressures in various scenarios.

[0005] A dynamic tracking adsorption testing device adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios includes a total reaction control unit, a self-regulating gas supply system, and a gas analysis system. The total reaction control unit is horizontally set, the gas inlet of the total reaction control unit is connected to the self-regulating gas supply system, and the gas outlet of the total reaction control unit is connected to the gas analysis system.

[0006] The self-regulating gas supply system includes an inert gas supply cylinder, a test gas supply cylinder, an adsorbed gas supply cylinder, a gas storage tank, a gas concentration detector, a humidity generator, a first mass flow controller, and a humidity sensor. The outlets of the inert gas supply cylinder, the test gas supply cylinder, and the adsorbed gas supply cylinder are respectively connected to the inlet of the gas storage tank. The humidity generator is connected to the gas storage tank through the first mass flow controller. The outlet of the gas storage tank is connected to the inlet of the total reaction control unit through the gas concentration detector and the humidity sensor.

[0007] As a preferred embodiment: the self-regulating gas supply system further includes a venting pipeline assembly, which includes a first venting pipe, a second venting pipe, a third venting pipe, a fourth venting pipe, a fifth venting pipe, and a sixth venting pipe. The outlet of the inert gas supply cylinder is connected to the inlet of the gas storage tank via the first venting pipe, and a first valve is installed on the first venting pipe. The outlet of the test gas supply cylinder is connected to the inlet of the gas storage tank via the second venting pipe, and a second valve is installed on the second venting pipe. The outlet of the adsorption gas supply cylinder is connected to the inlet of the gas storage tank via the third venting pipe, and a valve is installed on the third venting pipe. A third valve is provided. The humidity generator is connected to the gas storage tank via a fourth vent pipe. A first mass flow controller and a fourth valve are installed on the fourth vent pipe. The fourth valve is located between the first mass flow controller and the gas storage tank. The gas storage tank and the main reaction control unit are connected via a fifth vent pipe. The gas concentration detector and humidity sensor are installed on the fifth vent pipe. A fifth valve is installed on the fifth vent pipe and is located near the main reaction control unit. The gas concentration detector is located near the gas storage tank. A sixth vent pipe connects the first vent pipe and the fifth vent pipe, and a sixth valve is installed on the sixth vent pipe.

[0008] As a preferred embodiment: the total reaction control system includes a weight sensor, a ceramic boat, a vacuum tube furnace, a three-way valve, and a vacuum pump. The vacuum tube furnace is horizontally positioned, and the weight sensor and the ceramic boat are located inside the vacuum tube furnace. The weight sensor is located at the bottom of the ceramic boat. The three-way valve is connected to the gas outlet of the vacuum tube furnace. One port of the three-way valve is connected to the vacuum tube furnace, and the other port of the three-way valve is connected to the vacuum pump.

[0009] As a preferred embodiment, the gas analysis system includes a gas analyzer, a computer acquisition system, and a bubble indicator. The third port of the three-way valve is connected to the bubble indicator through the gas analyzer, and the gas analyzer is electrically connected to the computer acquisition system.

[0010] A dynamic tracking adsorption test method adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios is disclosed. This method utilizes the aforementioned dynamic tracking adsorption test device adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios. The dynamic tracking adsorption test method involves pre-treating the test sample under vacuum activation, followed by adsorption and desorption, and obtaining the mass change and inlet / outlet concentration data during the adsorption stage. A triple adsorption capacity calculation model is established based on the mass change and inlet / outlet concentration data during the adsorption stage. The adsorption cycle stability test process is then completed based on the triple adsorption capacity calculation model after data analysis.

[0011] As a preferred option, the test sample is inspected before vacuum activation pretreatment. The inspection includes checking the sealing performance and connection status of the total reaction control system, the self-regulating gas supply system, and the gas analysis system.

[0012] As a preferred option, the vacuum activation pretreatment process for the test sample is as follows: Place the test sample in a ceramic boat, ensuring that the test sample is evenly distributed on the ceramic boat with a thickness of 1~5mm; place the ceramic boat containing the test sample on the weight sensor in the vacuum tube furnace, ensuring that the ceramic boat and the weight sensor are on the same vertical central axis; close the inlet of the vacuum tube furnace to ensure that the inside of the vacuum tube furnace is in a sealed state, then close the three-way valve, start the vacuum pump, and ensure that the vacuum tube furnace reaches the predetermined vacuum state before starting the heating function of the vacuum tube furnace to carry out the vacuum activation process. After the vacuum activation process is completed, close the three-way valve connected to the vacuum pump, and start the gas analyzer to test the adsorption process of removing the adsorbent's pre-adsorption of impurity gases.

[0013] As a preferred approach, the process of obtaining mass change and inlet / outlet concentration data during the adsorption stage after vacuum activation pretreatment of the test sample, followed by adsorption and desorption, is as follows:

[0014] Adsorption process: First, open the first valve at the inert gas supply cylinder and the second valve at the test gas supply cylinder to ensure that the inert gas supply cylinder is connected to the vacuum tube furnace through the first vent pipe and the test gas supply cylinder is connected to the storage tank through the second vent pipe. Zero the reading of the weight sensor and adjust the first mass flow controller according to the predetermined gas partial pressure requirements. Mix the gas at a flow rate of 0.1~0.5L / min and introduce it into the storage tank to form a mixed gas. When there is a corresponding requirement to adjust the gas humidity, turn on the humidity generator and adjust the flow rate of saturated water vapor entering the storage tank to meet the predetermined requirements by adjusting the first mass flow controller. When the corresponding values ​​of the gas concentration detector and humidity sensor meet the predetermined requirements, open the fourth valve to allow the gas flow in the storage tank to flow into the vacuum tube furnace at a flow rate of 0.5~1.0L / min. After the mixed gas is filled into the vacuum tube furnace, observe the changes in the readings of the weight sensor and gas analyzer simultaneously. Complete the adsorption process accompanied by the mixed gas within the predetermined time.

[0015] The concentration of carbon dioxide gas introduced into the vacuum tube furnace is measured by a gas concentration detector, and the concentration of carbon dioxide gas discharged from the vacuum tube furnace is measured by a gas analyzer. The adsorption capacity of the adsorbent is calculated based on the change in carbon dioxide concentration in the incoming and outgoing gases. When the weight sensor reading is stable and the gas concentration before and after the vacuum tube furnace test is consistent, it indicates that the adsorption capacity has reached saturation, that is, the test sample has reached the maximum adsorption capacity. When the carbon dioxide concentration discharged from the vacuum tube furnace is 5% of the carbon dioxide concentration introduced into the vacuum tube furnace, the carbon dioxide adsorption capacity of the test sample at this time is the breakthrough adsorption capacity.

[0016] Desorption process: Simultaneously open the first valve and the sixth valve, close the gas storage tank, and after the gas analyzer reading is zero, stabilize the gas flow rate supplied by the inert gas supply cylinder at 0.1~0.5L / min. Set the corresponding desorption reaction time and temperature according to the test requirements, and turn on the vacuum tube furnace for heating. The computer acquisition system acquires and records the carbon dioxide content data displayed in real time by the gas analyzer until the value changes from the beginning to zero and remains unchanged for the predetermined time period, indicating that the desorption reaction is over.

[0017] Data analysis process: Based on the mass change during the adsorption stage and the integral data of inlet and outlet concentrations, a triple adsorption capacity calculation model was established. q 1. q 2. q 3) The corresponding formulas are Formula 1, Formula 2, and Formula 3, respectively:

[0018] Formula 1

[0019] In the above formula, q1 represents the amount of gas adsorbed during the adsorption stage, in cm³.3 / g; w is the weight of the adsorbent material in g; t0 and t1 are the start and end times for the adsorbent material to desorb and show readings, respectively, in min; Q is the fixed flow rate during inert gas purging, in mL / min; C is the real-time reading of the gas analyzer at the outlet of the tubular furnace, in %; C0 is the reading of the gas concentration meter at the inlet of the tubular furnace, in %; V m The value represents the molar volume of the adsorbed gas, expressed in mL / mmol.

[0020] Formula 2

[0021] In the above formula, q2 represents the amount of gas adsorbed during the desorption phase, in cm³. 3 / g, w is the weight of the adsorbent material in g, t0 and t1 are the start and end times when the adsorbent material shows readings during desorption in min, Q is the fixed flow rate during inert gas purging in mL / min; C t This is the real-time reading of the gas analyzer, in units of %; V m The value represents the molar volume of the adsorbed gas, expressed in mL / mmol.

[0022] Formula 3

[0023] In the above formula, q3 represents the amount of gas adsorbed during the adsorption stage, in cm³. 3 / g; w is the weight of the adsorbent material in g; ∆G is the change in the reading of the weight sensor before and after, in g; M is the molar mass of carbon dioxide in g / mol;

[0024] Based on three calculation models, until the final result is reached This indicates that the acquired data is reliable and can be used for subsequent purposes.

[0025] As a preferred method, the adsorption cycle stability test process based on the triple adsorption capacity calculation model after data analysis is as follows: After completing the adsorption experiment, simultaneously open the first and sixth valves, and pass the inert gas through the vacuum tube furnace at a predetermined flow rate of 0.1~0.5 L / min. Set the temperature and time, and the desorption reaction begins. Observe the carbon dioxide concentration reading on the gas analyzer. After the value appears and then returns to 0 and remains unchanged for a predetermined time, it indicates that the desorption reaction is over. At this time, after the temperature of the tube furnace drops to the adsorption temperature, open the second valve and close the sixth valve simultaneously. Adjust the flow rate according to the predetermined gas partial pressure and introduce it into the gas storage tank, so that the mixed gas with the predetermined carbon dioxide concentration flows in, and the adsorption reaction begins. Repeat the above steps, and the cycle stability of the adsorbent can be judged by the change in adsorption capacity with the number of cycles. When the adsorption capacity remains unchanged or decreases slowly with the number of cycles by no more than 10%, it indicates that the cycle stability of the adsorbent is in a good state. When the adsorption capacity decreases rapidly with the number of cycles and drops to 0 after at least three cycles, it indicates that the cycle stability of the adsorbent is in a failed state.

[0026] As a preferred approach, when the adsorption capacity disappears to 0 within seconds with increasing number of cycles, it also indicates that the cyclic stability of the adsorbent is in a state of failure.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] The dynamic tracking adsorption testing device of this invention, adaptable to various scenarios and different carbon dioxide partial pressures of adsorbents, constructs a high-precision, multi-scenario adaptable adsorption performance testing system through the coordinated operation of a total reaction control unit, a gas analysis system, and a self-regulating gas supply system consisting of an inert gas supply bottle, a test gas supply bottle, an adsorbed gas supply bottle, a gas storage tank, a gas concentration detector, a humidity generator, a first mass flow controller, and a humidity sensor. This system can test the adsorption performance, desorption performance, and cycle stability of solid adsorbents under different gas partial pressures, flow rates, humidity, and temperature conditions, forming a continuous and accurate acquisition process for these three properties. This invention enables cross-validation of adsorption capacity through mass-concentration dual-modal sensing, providing comprehensive data support for material optimization and engineering applications.

[0029] The dynamic tracking adsorption testing method of this invention, adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in various scenarios, provides a more comprehensive, efficient, and economical solution for testing the gas adsorption capacity of materials. By integrating a vacuum activation system, a standardized and continuous processing procedure can be formed, and the vacuum high-temperature activation process can be completed in a standardized manner, eliminating measurement deviations caused by adsorbed impurities on the material surface. Through the cooperation of the vacuum tube furnace, weight sensor, ceramic boat, gas analysis system, and self-regulating gas supply system, the dynamic response of material mass change and gas concentration can be monitored synchronously. Through the flow meter and gas analyzer, data such as adsorption amount and adsorption rate can be obtained, thereby accurately calculating the adsorption efficiency, providing guidance for the standardized processing of adsorbents with different carbon dioxide partial pressure adsorption performance in various scenarios through dynamic tracking adsorption testing. Attached Figure Description

[0030] Figure 1 A schematic diagram of a dynamic tracking adsorption testing device adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in various scenarios;

[0031] Figure 2 This is a schematic diagram of the main structure of the venting piping assembly.

[0032] Figure 3 This is a schematic diagram of the main structure of the overall control panel.

[0033] In the diagram, 1-total reaction control unit; 1-1-weight sensor; 1-2-ceramic boat; 1-3-vacuum tube furnace; 1-4-three-way valve; 1-5-vacuum pump; 2-1-inert gas supply bottle; 2-2-test gas supply bottle; 2-3-adsorbent gas supply bottle; 2-4-gas storage tank; 2-5-gas concentration detector; 2-6-humidity generator; 2-7-first mass flow controller; 2-8-humidity sensor; 3-first vent pipe; 4-second vent pipe; 5-third vent pipe; 6-fourth vent pipe; 7-fifth vent pipe; 8-sixth vent pipe; 9-first valve; 10-second valve; 11-third valve; 12-fourth valve; 13-fifth valve; 14-gas analyzer; 15-computer data acquisition system; 16-bubble indicator; 20-sixth valve; 22-second mass flow controller; 23-third mass flow controller; 24-fourth mass flow controller. Detailed Implementation

[0034] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. 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.

[0035] Specific implementation method one: Combining Figure 1 , Figure 2 and Figure 3 This embodiment describes a dynamic tracking adsorption testing device adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios. It includes a total reaction control unit 1, a self-regulating gas supply system, and a gas analysis system. The total reaction control unit 1 is horizontally positioned, with its inlet connected to the self-regulating gas supply system and its outlet connected to the gas analysis system.

[0036] The self-regulating gas supply system includes an inert gas supply cylinder 2-1, a test gas supply cylinder 2-2, an adsorbed gas supply cylinder 2-3, a gas storage tank 2-4, a gas concentration detector 2-5, a humidity generator 2-6, a first mass flow controller 2-7, and a humidity sensor 2-8. The outlets of the inert gas supply cylinder 2-1, the test gas supply cylinder 2-2, and the adsorbed gas supply cylinder 2-3 are respectively connected to the inlet of the gas storage tank 2-4. The humidity generator 2-6 is connected to the gas storage tank 2-4 through the first mass flow controller 2-7. The outlet of the gas storage tank 2-4 is connected to the inlet of the total reaction control unit 1 through the gas concentration detector 2-5 and the humidity sensor 2-8.

[0037] In this embodiment, test gas supply bottle 2-2 is used to provide carbon dioxide gas, and adsorption gas supply bottle 2-3 is used to provide gas supply for the detection of other gases. Adsorption gas supply bottle 2-3 can also be used as a backup gas source for the detection of the same gas.

[0038] In this embodiment, the first mass flow controller 2-7 is an MFC first mass flow controller, which is an existing first mass flow controller with an accuracy of ±0.5%FS and a range of 0-1000mL / min.

[0039] Specific Implementation Method Two: This implementation method is a further limitation of Specific Implementation Method One. In this implementation method, the self-regulating gas supply system also includes a gas pipeline assembly. The gas pipeline assembly includes a first gas pipe 3, a second gas pipe 4, a third gas pipe 5, a fourth gas pipe 6, a fifth gas pipe 7, and a sixth gas pipe 8. The outlet of the inert gas supply cylinder 2-1 is connected to the inlet of the gas storage tank 2-4 through the first gas pipe 3. A first valve 9 is provided on the first gas pipe 3. A second valve 8 is provided on the first gas pipe 3. A second mass flow controller 22 is used to quantify and control the airflow rate in the first vent pipe 3. The outlet of the test gas supply cylinder 2-2 is connected to the inlet of the storage tank 2-4 through the second vent pipe 4. A second valve 10 is installed on the second vent pipe 4. A third mass flow controller 23 is installed on the second vent pipe 4 to quantify and control the airflow rate in the second vent pipe 4. The outlet of the adsorption gas supply cylinder 2-3 is connected to the inlet of the storage tank 2-4 through the third vent pipe 5. A third valve 11 is installed on the third vent pipe 5. A fourth mass flow controller 24 is installed on the third vent pipe 5 to quantify and control the airflow rate in the third vent pipe 5. A humidity generator 2-6 is connected to the storage tank 2-4 through the fourth vent pipe 6. A first mass flow controller 2-7 and a fourth valve 12 are installed on the fourth vent pipe 6. The fourth valve 12 is located on the first mass flow controller 2-7. The gas storage tank 2-4 and the main reaction control unit 1 are connected by a fifth vent pipe 7. The gas concentration detector 2-5 and the humidity sensor 2-8 are installed on the fifth vent pipe 7. The fifth valve 13 is installed on the fifth vent pipe 7 and is located near the main reaction control unit 1. The gas concentration detector 2-5 is located near the gas storage tank 2-4. A sixth vent pipe 8 is connected between the first vent pipe 3 and the fifth vent pipe 7. The sixth vent pipe 8 is equipped with a sixth valve 20.

[0040] In this embodiment, each mass flow controller is an existing flow controller, and its working principle is the same as that of existing flow controllers.

[0041] Furthermore, the first mass flow controller 2-7, the second mass flow controller 22, the third mass flow controller 23, and the fourth mass flow controller 24 are all electrically connected to the gas analysis system to provide feedback on the flow data of each ventilation path.

[0042] Specific Implementation Method 3: This implementation method is a further limitation of Specific Implementation Method 1 or 2. In this implementation method, the total reaction control system 1 includes a weight sensor 1-1, a ceramic boat 1-2, a vacuum tube furnace 1-3, a three-way valve 1-4, and a vacuum pump 1-5. The vacuum tube furnace 1-3 is horizontally arranged. The weight sensor 1-1 and the ceramic boat 1-2 are arranged inside the vacuum tube furnace 1-3. The weight sensor 1-1 is arranged at the bottom of the ceramic boat 1-2. The three-way valve 1-4 is connected to the gas outlet of the vacuum tube furnace 1-3. One port of the three-way valve 1-4 is connected to the vacuum tube furnace 1-3, and the other port of the three-way valve 1-4 is connected to the vacuum pump 1-5.

[0043] In this embodiment, the weight sensor 1-1 is an existing weight sensor, and its working principle is the same as that of existing weight sensors. Its range is 0-100g and its resolution is 0.01mg.

[0044] Specific Implementation Method 4: This implementation method is a further limitation of Specific Implementation Method 1, 2 or 3. In this implementation method, the gas analysis system includes a gas analyzer 14, a computer acquisition system 15 and a bubble indicator 16. The third connection port of the three-way valve 1-4 is connected to the bubble indicator 16 through the gas analyzer 14, and the gas analyzer 14 is electrically connected to the computer acquisition system 15.

[0045] This device mixes dry gas and saturated water vapor in a specific ratio. The flow rate ratio of the saturated water vapor is precisely adjusted by the first mass flow controller 2-7 to achieve the target humidity.

[0046] Specific Implementation Method Five: Combining Figure 1 As shown in the figure, the dynamic tracking adsorption test method adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios in this embodiment is implemented using a dynamic tracking adsorption test device adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios. In this embodiment, the dynamic tracking adsorption test method involves pre-treating the test sample under vacuum activation, then performing adsorption and desorption to obtain the mass change and inlet / outlet concentration data during the adsorption stage. Based on the mass change and inlet / outlet concentration data during the adsorption stage, a triple adsorption capacity calculation model is established. The adsorption cycle stability test process is completed based on the triple adsorption capacity calculation model after data analysis.

[0047] The dynamic tracking adsorption testing device in this embodiment includes a total reaction control unit 1, a self-regulating gas supply system, and a gas analysis system. The total reaction control unit 1 is horizontally arranged, the gas inlet of the total reaction control unit 1 is connected to the self-regulating gas supply system, and the gas outlet of the total reaction control unit 1 is connected to the gas analysis system.

[0048] The self-regulating gas supply system includes an inert gas supply cylinder 2-1, a test gas supply cylinder 2-2, an adsorbed gas supply cylinder 2-3, a gas storage tank 2-4, a gas concentration detector 2-5, a humidity generator 2-6, a first mass flow controller 2-7, and a humidity sensor 2-8. The outlets of the inert gas supply cylinder 2-1, the test gas supply cylinder 2-2, and the adsorbed gas supply cylinder 2-3 are respectively connected to the inlet of the gas storage tank 2-4. The humidity generator 2-6 is connected to the gas storage tank 2-4 through the first mass flow controller 2-7. The outlet of the gas storage tank 2-4 is connected to the inlet of the total reaction control unit 1 through the gas concentration detector 2-5 and the humidity sensor 2-8.

[0049] The self-regulating gas supply system also includes a first vent pipe 3, a second vent pipe 4, a third vent pipe 5, a fourth vent pipe 6, a fifth vent pipe 7, and a sixth vent pipe 8. The outlet of the inert gas supply cylinder 2-1 is connected to the inlet of the storage tank 2-4 via the first vent pipe 3, and a first valve 9 is installed on the first vent pipe 3. The outlet of the test gas supply cylinder 2-2 is connected to the inlet of the storage tank 2-4 via the second vent pipe 4, and a second valve 10 is installed on the second vent pipe 4. The outlet of the adsorption gas supply cylinder 2-3 is connected to the inlet of the storage tank 2-4 via the third vent pipe 5, and a third valve 11 is installed on the third vent pipe 5. The humidity generator 2-6 is connected to the fourth vent pipe 8. Ventilation pipe 6 is connected to gas storage tank 2-4. A first mass flow controller 2-7 and a fourth valve 12 are installed on the fourth ventilation pipe 6. The fourth valve 12 is located between the first mass flow controller 2-7 and gas storage tank 2-4. Gas storage tank 2-4 and reaction control unit 1 are connected by a fifth ventilation pipe 7. The gas concentration detector 2-5 and humidity sensor 2-8 are installed on the fifth ventilation pipe 7. A fifth valve 13 is installed on the fifth ventilation pipe 7 and is located near the reaction control unit 1. The gas concentration detector 2-5 is located near the gas storage tank 2-4. A sixth ventilation pipe 8 is connected between the first ventilation pipe 3 and the fifth ventilation pipe 7. A sixth valve 20 is installed on the sixth ventilation pipe 8.

[0050] The reaction control unit 1 includes a weight sensor 1-1, a ceramic boat 1-2, a vacuum tube furnace 1-3, a three-way valve 1-4, and a vacuum pump 1-5. The vacuum tube furnace 1-3 is horizontally positioned. The weight sensor 1-1 and the ceramic boat 1-2 are located inside the vacuum tube furnace 1-3. The weight sensor 1-1 is located at the bottom of the ceramic boat 1-2. The three-way valve 1-4 is connected to the gas outlet of the vacuum tube furnace 1-3. One port of the three-way valve 1-4 is connected to the vacuum tube furnace 1-3, and the other port of the three-way valve 1-4 is connected to the vacuum pump 1-5.

[0051] The gas analysis system includes a gas analyzer 14, a computer acquisition system 15, and a bubble indicator 16. The third port of the three-way valve 1-4 is connected to the bubble indicator 16 through the gas analyzer 14, and the gas analyzer 14 is electrically connected to the computer acquisition system 15.

[0052] Specific Implementation Method Six: This implementation method is a further limitation of Specific Implementation Method Five. In this implementation method, the test sample is inspected before vacuum activation pretreatment. The inspection operation is to check the sealing performance and connection status of the total reaction control unit 1, the self-regulating gas supply system and the gas analysis system.

[0053] Specific Implementation Method Seven: This implementation method is a further limitation of Specific Implementation Method Six or Seven. In this implementation method, the process of vacuum activation pretreatment of the test sample is as follows: The test sample is placed in the ceramic boat 1-2, ensuring that the test sample is evenly distributed in the ceramic boat 1-2 with a thickness of 1~5mm; the ceramic boat 1-2 containing the test sample is placed on the weight sensor 1-1 in the vacuum tube furnace 1-3, ensuring that the ceramic boat 1-2 and the weight sensor 1-1 are on the same vertical central axis; the inlet of the vacuum tube furnace 1-3 is closed to ensure that the inside of the vacuum tube furnace 1-3 is in a sealed state, and then the three-way valve 1-4 is closed. The vacuum pump 1-5 is started, and the vacuum pump 1-5 ensures that the vacuum tube furnace 1-3 reaches the predetermined vacuum state before starting the heating function of the vacuum tube furnace 1-3 to carry out the vacuum activation treatment process. After the vacuum activation treatment process is completed, the three-way valve 1-4 connected to the vacuum pump 1-5 is closed, and the gas analyzer 14 is started to test the adsorption process of removing the adsorbent's pre-adsorption of impurity gases.

[0054] Specific Implementation Method Eight: This implementation method is a further limitation of Specific Implementation Methods Five, Six, or Seven. In this implementation method, the process of obtaining the mass change and inlet / outlet concentration data of the adsorption stage after the test sample undergoes vacuum activation pretreatment, adsorption, and desorption is as follows:

[0055] Adsorption process: First, open the first valve 9 at the inert gas supply cylinder 2-1 and the second valve 10 at the test gas supply cylinder 2-2, ensuring that the inert gas supply cylinder 2-1 is connected to the vacuum tube furnace 1-3 via the first vent pipe 3, and that the test gas supply cylinder 2-2 is connected to the gas storage tank 2-4 via the second vent pipe 4. Zero the reading of the weight sensor 1-1, and adjust the first mass flow controller 2-7 according to the predetermined gas partial pressure requirements. Mix the gases at a flow rate of 0.1~0.5L / min in the corresponding proportion to form a mixed gas, which is then introduced into the gas storage tank 2-4. When the predetermined requirements include adjusting the gas humidity... When required, the humidity generator 2-6 is turned on, and the flow rate of saturated water vapor entering the gas storage tank 2-4 is controlled by adjusting the first mass flow controller 2-7 to reach the predetermined requirement; when the corresponding values ​​of the gas concentration detector 2-5 and the humidity sensor 2-8 meet the predetermined requirements, the fourth valve 12 is opened, so that the airflow in the gas storage tank 2-4 flows into the vacuum tube furnace 1-3 at a flow rate of 0.5~1.0L / min. After the mixed gas is filled into the vacuum tube furnace 1-3, the reading changes of the weight sensor 1-1 and the gas analyzer 14 are observed simultaneously, and the adsorption process accompanied by the mixed gas is completed within the predetermined time.

[0056] The concentration of carbon dioxide gas introduced into the vacuum tube furnace 1-3 is measured by a gas concentration detector 2-5, and the concentration of carbon dioxide gas discharged from the vacuum tube furnace 1-3 is measured by a gas analyzer 14. The adsorption capacity of the adsorbent is calculated based on the change in carbon dioxide concentration in the incoming and outgoing gases. When the reading of the weight sensor 1-1 is stable and the gas concentration before and after the test in the vacuum tube furnace 1-3 is consistent, it indicates that the adsorption capacity has reached saturation, that is, the test sample has reached the maximum adsorption capacity. When the carbon dioxide concentration discharged from the vacuum tube furnace 1-3 is 5% of the carbon dioxide concentration introduced into the vacuum tube furnace 1-3, the carbon dioxide adsorption capacity of the test sample at this time is the breakthrough adsorption capacity.

[0057] Desorption process: Simultaneously open the first valve 9 and the sixth valve 20, close the gas storage tank 2-4, and when the reading of the gas analyzer 14 is zero, stabilize the flow rate of the gas supplied by the inert gas supply cylinder 2-1 at 0.1~0.5L / min. Then, set the corresponding desorption reaction time and temperature according to the test requirements, turn on the vacuum tube furnace 1-3 for heating, and the computer acquisition system 15 acquires the carbon dioxide content data displayed in real time by the gas analyzer 14 and records it until the value changes back to 0 and remains unchanged for a predetermined time period, indicating that the desorption reaction is over.

[0058] The desorption reaction time was set to 60 min and the desorption reaction temperature to 130℃ according to the experimental requirements. The time and temperature can be determined according to the specific desorption requirements.

[0059] Data analysis process: Based on the mass change during the adsorption stage and the integral data of inlet and outlet concentrations, a triple adsorption capacity calculation model was established. q 1. q 2. q 3. The corresponding formulas are Formula 1, Formula 2, and Formula 3:

[0060] Formula 1

[0061] In the above formula, q1 represents the amount of gas adsorbed during the adsorption stage, in cm³. 3 / g; w is the weight of the adsorbent material in g; t0 and t1 are the start and end times for the adsorbent material to desorb and show readings, respectively, in min; Q is the fixed flow rate during inert gas purging, in mL / min; C is the real-time reading of the gas analyzer 14 at the outlet of the tubular furnace, in %; C0 is the reading of the gas concentration meter at the inlet of the tubular furnace, in %; V m The value represents the molar volume of the adsorbed gas, expressed in mL / mmol.

[0062] Formula 2

[0063] In the above formula, q2 represents the amount of gas adsorbed during the desorption phase, in cm³. 3 / g, w is the weight of the adsorbent material in g, t0 and t1 are the start and end times when the adsorbent material shows readings during desorption in min, Q is the fixed flow rate during inert gas purging in mL / min; C t The readings of gas analyzer 14 are real-time values, expressed in %; V m The value represents the molar volume of the adsorbed gas, expressed in mL / mmol.

[0064] Formula 3

[0065] In the above formula, q3 represents the amount of gas adsorbed during the adsorption stage, in cm³. 3 / g; w is the weight of the adsorbent material in g; ∆G is the change in the reading of the weight sensor before and after step 1-1 in g; M is the molar mass of carbon dioxide in g / mol;

[0066] Based on three calculation models, until the final result is reached This indicates that the acquired data is reliable and can be used for subsequent purposes.

[0067] Specific Implementation Method Nine: This implementation method is a further limitation of Specific Implementation Methods Five, Six, Seven, or Eight. In this implementation method, the adsorption cycle stability test process based on the triple adsorption capacity calculation model after data analysis is as follows: After the adsorption experiment is completed, the first valve 9 and the sixth valve 20 are opened simultaneously, and the inert gas is passed through the vacuum tube furnace 1-3 at a predetermined flow rate of 0.1~0.5 L / min. The temperature and time are set, and the desorption reaction begins. The carbon dioxide concentration reading on the gas analyzer 14 is observed. After the value initially appears and then returns to 0 and remains unchanged for a predetermined time, it indicates that the desorption reaction is over. At this time, after the temperature of the tube furnace drops to the adsorption temperature, the second valve 10 is opened and the sixth valve 20 is closed simultaneously. The flow rate is adjusted according to the predetermined gas partial pressure and introduced into the gas storage tank 2-4, so that the mixed gas with the predetermined carbon dioxide concentration flows in, and the adsorption reaction begins. By repeating the above steps, the cycling stability of the adsorbent can be determined by observing the change in adsorption capacity over the number of cycles. When the adsorption capacity remains constant or decreases slowly by no more than 10% with increasing cycles, it indicates that the cycling stability of the adsorbent is in good condition. When the adsorption capacity decreases rapidly with increasing cycles and drops to 0 after at least three cycles, it indicates that the cycling stability of the adsorbent is in failure.

[0068] Another way to determine the failure state of the cyclic stability of the adsorbent in this embodiment is that when the adsorption capacity disappears to 0 within a few seconds as the number of cycles increases, it also indicates that the cyclic stability of the adsorbent is in a failure state.

[0069] Specific Implementation Method 10: This implementation method is a further limitation of Specific Implementation Methods 5, 6, 7, 8 or 9. In this implementation method, when harmful gases such as CO and CH4 are involved in the process of promoting this method, an exhaust gas treatment device needs to be installed at the outlet. The working principle of the exhaust gas treatment device is the same as that of the existing exhaust gas treatment device.

Claims

1. A dynamic tracking adsorption testing device adapted to the adsorption performance of adsorbents with different carbon dioxide partial pressures in various scenarios, characterized in that: It includes a total reaction control unit (1), a self-regulating gas supply system and a gas analysis system. The total reaction control unit (1) is set horizontally. The gas inlet of the total reaction control unit (1) is connected to the self-regulating gas supply system, and the gas outlet of the total reaction control unit (1) is connected to the gas analysis system. The self-regulating gas supply system includes an inert gas supply cylinder (2-1), a test gas supply cylinder (2-2), an adsorbed gas supply cylinder (2-3), a gas storage tank (2-4), a gas concentration detector (2-5), a humidity generator (2-6), a first mass flow controller (2-7), and a humidity sensor (2-8). The outlet of the inert gas supply cylinder (2-1), the outlet of the test gas supply cylinder (2-2), and the outlet of the adsorbed gas supply cylinder (2-3) are respectively connected to the inlet of the gas storage tank (2-4). The humidity generator (2-6) is connected to the gas storage tank (2-4) through the first mass flow controller (2-7). The outlet of the gas storage tank (2-4) is connected to the inlet of the reaction control unit (1) through the gas concentration detector (2-5) and the humidity sensor (2-8). The self-regulating gas supply system further includes a first vent pipe (3), a second vent pipe (4), a third vent pipe (5), a fourth vent pipe (6), a fifth vent pipe (7), and a sixth vent pipe (8). The outlet of the inert gas supply cylinder (2-1) is connected to the inlet of the gas storage tank (2-4) through the first vent pipe (3). A first valve (9) is provided on the first vent pipe (3). The outlet of the test gas supply cylinder (2-2) is connected to the inlet of the gas storage tank (2-4) through the second vent pipe (4). A second valve (10) is provided on the second vent pipe (4). The outlet of the adsorbent gas supply cylinder (2-3) is connected to the inlet of the gas storage tank (2-4) through the third vent pipe (5). A third valve (11) is provided on the third vent pipe (5). The humidity generator (2-6) is connected to the fourth vent pipe. (6) Connected to the gas storage tank (2-4), the fourth vent pipe (6) is equipped with a first mass flow controller (2-7) and a fourth valve (12), the fourth valve (12) is located between the first mass flow controller (2-7) and the gas storage tank (2-4), the gas storage tank (2-4) and the reaction control unit (1) are connected through a fifth vent pipe (7), the fifth vent pipe (7) is equipped with the gas concentration detector (2-5) and a humidity sensor (2-8), the fifth vent pipe (7) is equipped with a fifth valve (13), the fifth valve (13) is located near the reaction control unit (1), the gas concentration detector (2-5) is located near the gas storage tank (2-4); the first vent pipe (3) and the fifth vent pipe (7) are connected by a sixth vent pipe (8), the sixth vent pipe (8) is equipped with a sixth valve (20); The overall control system (1) includes a weight sensor (1-1), a ceramic boat (1-2), a vacuum tube furnace (1-3), a three-way valve (1-4), and a vacuum pump (1-5). The vacuum tube furnace (1-3) is horizontally positioned. The weight sensor (1-1) and the ceramic boat (1-2) are located inside the vacuum tube furnace (1-3). The weight sensor (1-1) is located at the bottom of the ceramic boat (1-2). The three-way valve (1-4) is connected to the outlet of the vacuum tube furnace (1-3). One port of the three-way valve (1-4) is connected to the vacuum tube furnace (1-3), and the other port of the three-way valve (1-4) is connected to the vacuum pump (1-5).

2. The dynamic tracking adsorption testing device for adapting to different carbon dioxide partial pressure adsorbents in multiple scenarios, as described in claim 1, is characterized in that: The gas analysis system includes a gas analyzer (14), a computer acquisition system (15), and a bubble indicator (16). The third port of the three-way valve (1-4) is connected to the bubble indicator (16) through the gas analyzer (14), and the gas analyzer (14) is electrically connected to the computer acquisition system (15).

3. A dynamic tracking adsorption test method adaptable to the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios, implemented using the dynamic tracking adsorption test device described in claim 1 or 2, characterized in that: The dynamic tracking adsorption test method involves pre-treating the test sample under vacuum activation, then performing adsorption and desorption to obtain mass change and inlet / outlet concentration data during the adsorption stage. Based on the mass change and inlet / outlet concentration data during the adsorption stage, a triple adsorption capacity calculation model is established. The adsorption cycle stability test process is then completed based on the triple adsorption capacity calculation model after data analysis. The triple adsorption capacity calculation models are: the adsorption capacity of the adsorbent calculated based on the change in carbon dioxide concentration in the incoming and outgoing gases during the adsorption process; the total amount of carbon dioxide desorbed from the sample during the desorption stage; and the adsorption capacity calculated by converting the increase in sample mass before and after adsorption during the adsorption stage.

4. The dynamic tracking adsorption test method for adapting the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios according to claim 3, characterized in that: Before the test sample was pretreated by vacuum activation, an inspection was performed. The inspection included checking the sealing performance and connection status of the total reaction control (1), the self-regulating gas supply system, and the gas analysis system.

5. The dynamic tracking adsorption test method for adapting the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios according to claim 3 or 4, characterized in that: The process of vacuum activation pretreatment of the test sample is as follows: the test sample is placed in a ceramic boat (1-2) to ensure that the test sample is evenly distributed in the ceramic boat (1-2) with a thickness of 1~5mm; the ceramic boat (1-2) containing the test sample is placed on the weight sensor (1-1) in the vacuum tube furnace (1-3) to ensure that the ceramic boat (1-2) and the weight sensor (1-1) are on the same vertical central axis; the inlet of the vacuum tube furnace (1-3) is closed to ensure that the inside of the vacuum tube furnace (1-3) is sealed, and then the three-way valve (1-4) is closed. The vacuum pump (1-5) is started. The vacuum pump (1-5) ensures that the vacuum tube furnace (1-3) reaches the predetermined vacuum state before starting the heating function of the vacuum tube furnace (1-3) to carry out the vacuum activation process. After the vacuum activation process is completed, the three-way valve (1-4) connected to the vacuum pump (1-5) is closed, and the gas analyzer (14) is started to carry out the test adsorption process of removing the adsorbent adsorbed impurity gas in the early stage.

6. The dynamic tracking adsorption test method for adapting the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios according to claim 5, characterized in that: The process of obtaining mass change and inlet / outlet concentration data during the adsorption stage after the test sample undergoes vacuum activation pretreatment, adsorption, and desorption is as follows: Adsorption process: First, open the first valve (9) at the inert gas supply cylinder (2-1) and the second valve (10) at the test gas supply cylinder (2-2) to ensure that the inert gas supply cylinder (2-1) is connected to the vacuum tube furnace (1-3) through the first vent pipe (3) and the test gas supply cylinder (2-2) is connected to the gas storage tank (2-4) through the second vent pipe (4). Zero the reading of the weight sensor (1-1) and adjust the first mass flow controller (2-7) according to the predetermined gas partial pressure requirements. Mix the gas at a flow rate of 0.1~0.5L / min according to the corresponding ratio to form a mixed gas and introduce it into the gas storage tank (2-4); when the predetermined requirements are met, adjust the gas moisture content. When the required humidity is met, the humidity generator (2-6) is turned on, and the flow rate of saturated water vapor entering the gas storage tank (2-4) is controlled by adjusting the first mass flow controller (2-7) to meet the predetermined requirements. When the corresponding values ​​of the gas concentration detector (2-5) and humidity sensor (2-8) meet the predetermined requirements, the fourth valve (12) is opened, so that the airflow in the gas storage tank (2-4) flows into the vacuum tube furnace (1-3) at a flow rate of 0.5~1.0L / min. After the mixed gas is filled into the vacuum tube furnace (1-3), the readings of the weight sensor (1-1) and gas analyzer (14) are observed simultaneously. The adsorption process accompanied by the mixed gas is completed within the predetermined time. The concentration of carbon dioxide gas in the vacuum tube furnace (1-3) is measured by a gas concentration detector (2-5), and the concentration of carbon dioxide gas discharged from the vacuum tube furnace (1-3) is measured by a gas analyzer (14). The adsorption capacity of the adsorbent is calculated based on the change in the concentration of carbon dioxide in the incoming and outgoing gases. When the reading of the weight sensor (1-1) is stable and the gas concentration before and after the test in the vacuum tube furnace (1-3) is consistent, it indicates that the adsorption capacity has reached the saturation state, that is, the test sample has reached the maximum adsorption capacity state. When the concentration of carbon dioxide discharged from the vacuum tube furnace (1-3) is 5% of the concentration of carbon dioxide in the vacuum tube furnace (1-3), it indicates that the carbon dioxide adsorption capacity of the test sample at this time is the breakthrough adsorption capacity. Desorption process: Open the first valve (9) and the sixth valve (20) at the same time, close the gas storage tank (2-4), and make the reading of the gas analyzer (14) zero. Then, stabilize the flow rate of the gas supplied by the inert gas supply bottle (2-1) at 0.1~0.5L / min. Set the corresponding desorption reaction time and temperature according to the test requirements and turn on the vacuum tube furnace (1-3) for heating. The computer acquisition system (15) acquires the carbon dioxide content data displayed in real time by the gas analyzer (14) and records it until the value appears from the beginning to return to 0 and remains unchanged for a predetermined time period, indicating that the desorption reaction is over. Data analysis process: Based on the mass change and inlet / outlet concentration integral data during the adsorption stage, a triple adsorption capacity calculation model was established, with corresponding formulas 1, 2, and 3: Formula 1 In the above formula, q1 represents the amount of gas adsorbed during the adsorption stage, in cm³. 3 / g; w is the weight of the adsorbent material, in grams; t0 and t1 are the start and end times of the adsorption process when the adsorbent material shows a reading, respectively, in min; Q is the fixed flow rate during inert gas purging, in mL / min; C is the real-time reading of the gas analyzer (14) at the outlet of the tubular furnace, in %; C0 is the reading of the gas concentration tester at the inlet of the tubular furnace, in %; V m The value represents the molar volume of the adsorbed gas, expressed in mL / mmol. Formula 2 In the above formula, q2 represents the amount of gas adsorbed during the desorption phase, in cm³. 3 / g, w is the weight of the adsorbent material in g, t0 and t1 are the start and end times when the adsorbent material shows readings during desorption in min, Q is the fixed flow rate during inert gas purging in mL / min; C t The real-time reading of the gas analyzer (14) is expressed in %; V m The value represents the molar volume of the adsorbed gas, expressed in mL / mmol. Formula 3 In the above formula, q3 represents the amount of gas adsorbed based on the mass adsorption stage, in cm³. 3 / g; w is the weight of the adsorbent material, in grams; V represents the change in the weight sensor reading before and after, in grams; M represents the molar mass of carbon dioxide, in g / mol; V m The value represents the molar volume of the adsorbed gas, expressed in mL / mmol. Based on three calculation models, until the final result is reached This indicates that the acquired data is reliable and can be used for subsequent purposes.

7. The dynamic tracking adsorption test method for adapting the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios according to claim 6, characterized in that: The adsorption cycle stability test process based on the triple adsorption capacity calculation model after data analysis is as follows: After completing the adsorption experiment, open the first valve (9) and the sixth valve (20) at the same time, and pass the inert gas through the vacuum tube furnace (1-3) at a predetermined flow rate of 0.1~0.5L / min. Set the temperature and time, and the desorption reaction begins. Observe the carbon dioxide concentration reading of the gas analyzer (14). After the value appears and then returns to 0 and remains unchanged for a predetermined time, it indicates that the desorption reaction is over. At this time, after the temperature of the tube furnace drops to the adsorption temperature, open the second valve (10) and close the sixth valve (20). Adjust the flow rate according to the predetermined gas partial pressure and introduce it into the gas storage tank (2-4) so ​​that the mixed gas with the predetermined carbon dioxide concentration flows in and the adsorption reaction begins. Repeat the above steps. By observing the change of adsorption capacity with the number of cycles, the cycle stability of the adsorbent can be judged. When the adsorption capacity remains unchanged or decreases slowly with the number of cycles by no more than 10%, it indicates that the cycle stability of the adsorbent is in good condition. When the adsorption capacity decreases rapidly with the number of cycles and drops to 0 after at least three cycles, it indicates that the cycle stability of the adsorbent is in failure.

8. The dynamic tracking adsorption test method for adapting the adsorption performance of adsorbents with different carbon dioxide partial pressures in multiple scenarios according to claim 7, characterized in that: When the adsorption capacity disappears to 0 within seconds with increasing number of cycles, it also indicates that the cyclic stability of the adsorbent is in a state of failure.

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