A method and system for automated control of catalytic reaction analysis instruments

Abstract

This application discloses an automated control method and system for a catalytic reaction analysis instrument, relating to the field of catalytic reaction analysis technology. The method includes the following steps: real-time acquisition of compositional data of reaction products; acquisition of catalyst activity indicators based on the compositional data; calculation of the rate of change of the activity indicators; during the reactor heating phase, when the rate of change exceeds a preset activation threshold, determining that an activity activation event is triggered, locking the reactor temperature at the temperature point at which the activity activation event is detected, and maintaining a preset isothermal duration; during the reactor isothermal operation phase, when the rate of change is less than a preset deactivation threshold, determining that a rapid deactivation event is triggered, increasing the flow rate of the feed gas to shorten the average residence time of the reaction products in the reactor; and increasing the frequency of compositional data acquisition in response to the determination of an activity activation event or a rapid deactivation event. This application can improve the adaptability of experiments, the effectiveness of data acquisition, and the accuracy of result interpretation.

Description

Technical Field

[0001] This application relates to the field of catalytic reaction analysis technology, and in particular to an automated control method and system for catalytic reaction analysis instruments. Background Technology

[0002] In the field of catalytic reaction analysis, automated control methods and systems are widely used to improve experimental efficiency and data reliability.

[0003] Existing automated control methods for catalytic reaction analysis instruments primarily rely on executing pre-set, fixed experimental program scripts. This approach is effective when dealing with catalysts whose behavior is known. However, it has significant limitations when conducting exploratory studies or long-term stability assessments of novel catalysts. Specifically, when catalysts exhibit unexpected behavior, such as sudden activation or deactivation, the system lacks the ability to respond in real time and autonomously adjust experimental strategies, often missing critical phenotype windows and resulting in insufficient data acquisition.

[0004] Furthermore, while the system can record catalyst performance changes during long-term operation, it cannot perform in-depth analysis and identification of the patterns of performance changes. Specifically, it cannot distinguish between intrinsic catalyst degradation and performance decline caused by external anomalies such as impurities in raw materials. This "knowing what happens, but not why" control logic prevents the system from proactively triggering diagnostic procedures or taking remedial measures when abnormal deactivation patterns are detected. This could lead to the failure of the entire experiment and a misjudgment of the catalyst's true performance. Summary of the Invention

[0005] This application proposes an automated control method and system for catalytic reaction analysis instruments, aiming to solve the technical problems of existing automated control methods for catalytic reaction analysis instruments when the reaction characteristics of the catalyst under test are unclear or long-term stability assessment is required. These problems include the possibility that the preset program may ignore key experimental phenomena, fail to respond in real time and adjust the experimental strategy autonomously, and fail to perform in-depth analysis and identification of performance change patterns, thus leading to experimental failure or misjudgment of the true performance of the catalyst.

[0006] In a first aspect, this application provides an automated control method for a catalytic reaction analysis instrument, used to control a gas-solid phase catalytic reaction process, wherein the gas-solid phase catalytic reaction process includes converting a feed gas into reaction products by passing it through a reactor containing a catalyst bed, and the method includes the following steps:

[0007] The composition data of the reaction products at the reactor outlet are acquired in real time, and the activity index of the catalyst is obtained based on the composition data.

[0008] The activity index is smoothed, and the rate of change of the processed activity index is periodically calculated.

[0009] When the reactor is in the heating phase according to a preset temperature-time curve, if the rate of change is greater than a preset activation threshold, an activation event is triggered, the heating phase is paused, the temperature of the reactor is locked at the temperature point at which the activation event was detected, and the temperature is maintained for a preset constant temperature duration; after the constant temperature duration ends, the paused heating phase is resumed starting from the temperature point.

[0010] When the reactor is in the isothermal operation stage, if the rate of change is less than a preset deactivation threshold, a rapid deactivation event is triggered, and the flow rate of the raw material gas is increased to shorten the average residence time of the reaction products in the reactor.

[0011] In response to the determination of the activity activation event or the rapid inactivation event, the frequency of acquiring the composition data is increased.

[0012] In some embodiments of this application, the step of acquiring compositional data of the reaction products at the reactor outlet in real time, and acquiring catalyst activity indicators based on the compositional data, includes:

[0013] The concentrations of each component of the reaction product at the reactor outlet are obtained using an online gas chromatograph installed in the reactor.

[0014] Based on the concentration of each component of the reaction products, the feed gas conversion rate or product selectivity is calculated as an indicator of catalyst activity.

[0015] In some embodiments of this application, the step of smoothing the activity index and periodically calculating the rate of change of the processed activity index includes:

[0016] The activity index is smoothed and filtered in real time using a moving average filtering algorithm.

[0017] Based on the processed activity index, the change in the activity index per unit time is calculated according to a preset time period, or the change in the activity index per unit temperature change is calculated according to a preset temperature change interval.

[0018] The change is taken as the rate of change of the activity index after processing.

[0019] In some embodiments of this application, when the reactor is in a heating phase according to a preset temperature-time curve, and the rate of change exceeds a preset activation threshold, an activation event is determined to be triggered, the heating phase is paused, the reactor temperature is locked at the temperature point at which the activation event was detected, and this is maintained for a preset isothermal duration; after the isothermal duration ends, the step of resuming the paused heating phase from the temperature point includes:

[0020] When the reactor is in the heating phase according to a preset temperature-time curve, if the rate of change is greater than a preset activation threshold, it is determined to be an activation event; wherein, the activation threshold is positive.

[0021] In response to the activity activation event, the temperature point at which the activity activation event is detected is recorded;

[0022] The temperature-time curve being executed is extended by adding a constant temperature segment starting from the time corresponding to the temperature point. The temperature of the constant temperature segment is the temperature point, and the duration of the constant temperature segment is the preset constant temperature duration, so as to pause the heating phase and lock the temperature of the reactor.

[0023] After the isothermal phase ends, the reactor is controlled to resume execution from the temperature point, resuming the portion of the temperature-time curve that follows the isothermal phase, in order to resume the suspended heating phase.

[0024] In some embodiments of this application, the step of adding a constant-temperature segment to the currently executing temperature-time curve, starting from the time corresponding to the temperature point, wherein the temperature of the constant-temperature segment is the temperature point, and the duration of the constant-temperature segment is a preset constant-temperature duration, to pause the heating phase and lock the reactor temperature includes:

[0025] The temperature-time curve currently being executed will be extended to include a constant temperature segment starting from the time corresponding to the temperature point, and an internal thermal management operation synchronized with the constant temperature segment will be initiated. The temperature of the constant temperature segment is the temperature point, and the duration of the constant temperature segment is the preset constant temperature duration.

[0026] The internal thermal management operation includes pre-cooling the feed gas, injecting inert gas into the feed gas, and starting a thermosiphon cycle to drive the inert gas to circulate within the catalyst bed to homogenize the temperature.

[0027] In some embodiments of this application, the step of determining that a rapid deactivation event is triggered when the rate of change is less than a preset deactivation threshold during the isothermal operation phase of the reactor, and increasing the flow rate of the feed gas to shorten the average residence time of the reaction products in the reactor, includes:

[0028] When the reactor is in a constant temperature operation phase, if the rate of change is less than a preset deactivation threshold, it is determined to be a rapid deactivation event; wherein, the deactivation threshold is negative.

[0029] In response to the rapid deactivation event, the set value of the gas mass flow controller installed on the inlet line of the reactor is increased to increase the flow rate of the feed gas, thereby reducing the average residence time of the reactants in the reactor by a preset adjustment ratio.

[0030] After changing the average residence time and maintaining the preset observation duration, the rate of change of the activity index is recalculated, and the inactive substance is judged.

[0031] In some embodiments of this application, the step of recalculating the rate of change of the activity index and determining the inactive substance after changing the average residence time and maintaining a preset observation duration includes:

[0032] After changing the average dwell time while maintaining the preset observation duration, the rate of change is recalculated;

[0033] If the recalculated rate of change is greater than or equal to the inactivation threshold after shortening the average residence time, it is preliminarily determined that the current inactivation has a tendency to be poisoned by impurities.

[0034] Based on the initial assessment that the current inactivation has a tendency to be poisoned by impurities, the current raw material gas source is switched to a backup high-purity raw material gas source, and the rate of change is monitored after the switch.

[0035] If the rate of change monitored after switching is greater than the preset attenuation threshold, then the rapid deactivation event is ultimately determined to be caused by impurities in the raw gas; wherein the attenuation threshold is negative and greater than the deactivation threshold.

[0036] In some embodiments of this application, the step of increasing the acquisition frequency of the composition data in response to determining that it is the activity activation event or the rapid inactivation event includes:

[0037] In response to the determination of the activity activation event or the rapid inactivation event, the absolute difference between the rate of change and the activation threshold or the inactivation threshold is calculated;

[0038] Based on the absolute difference, a frequency increase value is determined, and the frequency increase value is positively correlated with the absolute difference.

[0039] The improved sampling frequency is obtained by adding the initial sampling frequency to the constituent data.

[0040] In some embodiments of this application, after the step of increasing the acquisition frequency of the composition data in response to determining that it is the activity activation event or the rapid inactivation event, the following step is further included:

[0041] Generate a record containing the timestamp of the activation event or the rapid deactivation event, the event type, the rate of change, and the relevant parameters and values ​​before and after the temperature lock, dwell time adjustment and acquisition frequency adjustment operations performed;

[0042] The records are stored in the reactor's experimental log for traceability.

[0043] Secondly, this application also provides an automated control system for a catalytic reaction analysis instrument, used to control a gas-solid phase catalytic reaction process, wherein the gas-solid phase catalytic reaction process includes converting a feed gas into reaction products by passing it through a reactor containing a catalyst bed, the system comprising:

[0044] The index acquisition module is used to acquire the composition data of the reaction products at the reactor outlet in real time, and to acquire the activity index of the catalyst based on the composition data.

[0045] The speed calculation module is used to smooth the activity index and periodically calculate the rate of change of the processed activity index.

[0046] The heating control module is used to determine that an activation event is triggered when the rate of change of the reactor exceeds a preset activation threshold during the heating phase of heating according to a preset temperature-time curve. The heating phase is then paused, and the temperature of the reactor is locked at the temperature point at which the activation event was detected, and maintained for a preset constant temperature duration. After the constant temperature duration ends, the paused heating phase is resumed starting from the temperature point.

[0047] The constant temperature control module is used to determine and trigger a rapid deactivation event when the rate of change is less than a preset deactivation threshold during the constant temperature operation phase of the reactor, thereby increasing the flow rate of the raw material gas to shorten the average residence time of the reaction products in the reactor.

[0048] A frequency adjustment module is used to increase the acquisition frequency of the component data in response to the determination of the active activation event or the rapid inactivation event.

[0049] The technical solution according to the embodiments of this application has at least the following beneficial effects:

[0050] This application introduces mechanisms such as real-time activity index monitoring, dynamic temperature locking, flow rate adjustment, and adaptive data acquisition frequency adjustment, enabling catalytic reaction analysis instruments to respond more intelligently and flexibly to the complex behavior of catalysts. This improves the adaptability of experiments, the effectiveness of data acquisition, and the accuracy of result judgment, providing strong technical support for the development and application of novel catalysts.

[0051] Additional aspects and advantages of this application will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of this application. Attached Figure Description

[0052] The accompanying drawings are used to provide a further understanding of the technical solutions of this application and constitute a part of the specification. They are used together with the embodiments of this application to explain the technical solutions of this application and do not constitute a limitation on the technical solutions of this application.

[0053] Figure 1 This is a flowchart illustrating an automated control method for a catalytic reaction analysis instrument, provided as an embodiment of this application.

[0054] Figure 2 This is a schematic diagram of the architecture of an automated control system for a catalytic reaction analysis instrument provided in an embodiment of this application. Detailed Implementation

[0055] To make the objectives, technical methods, and advantages of this application clearer, the following detailed description is provided in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the scope of this application.

[0056] The technical solutions of this application will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are merely some embodiments of this application, and not all embodiments. The components of this application described and shown in the accompanying drawings can generally be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of this application provided in the accompanying drawings is not intended to limit the scope of the claimed application, but merely to illustrate selected embodiments of this application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

[0057] It should be noted that similar reference numerals and letters in the following figures indicate similar items; therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures. Furthermore, in the description of this application, terms such as "first," "second," etc., are used only to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0058] In the field of catalytic reaction analysis, traditional automated control methods mainly rely on preset fixed programs, which perform adequately when dealing with known catalysts. However, when faced with exploratory studies of novel catalysts or long-term stability assessments, these methods often struggle to adapt, failing to respond in real time to unexpected catalyst behaviors, such as sudden activation or deactivation. This can lead to missed key experimental phenomena, insufficient data acquisition, or biased assessments of catalyst performance. Furthermore, existing systems struggle to perform in-depth analysis of catalyst performance change patterns during long-term operation, failing to distinguish between intrinsic degradation and performance decline caused by external anomalies (such as impure feedstocks or reactor blockage). This results in the inability to proactively trigger diagnostic or remedial measures, potentially leading to experimental failures or misjudgments of the catalyst's true performance.

[0059] In this regard, such as Figure 1 As shown, this application discloses an automated control method for a catalytic reaction analysis instrument, used to control a gas-solid phase catalytic reaction process. The gas-solid phase catalytic reaction process includes converting a feed gas into reaction products by passing it through a reactor containing a catalyst bed. The method includes the following steps:

[0060] S110, acquire the composition data of the reaction products at the reactor outlet in real time, and acquire the activity index of the catalyst based on the composition data;

[0061] S120, the activity index is smoothed, and the rate of change of the processed activity index is periodically calculated.

[0062] S130, when the reactor is in the heating stage according to the preset temperature-time curve, if the rate of change is greater than the preset activation threshold, an activation event is determined to be triggered, the heating stage is paused, the temperature of the reactor is locked at the temperature point when the activation event is detected, and the preset constant temperature duration is maintained; after the constant temperature duration ends, the paused heating stage is resumed starting from the temperature point.

[0063] S140, when the reactor is in the constant temperature operation stage, if the rate of change is less than the preset deactivation threshold, a rapid deactivation event is triggered, and the flow rate of the raw material gas is increased to shorten the average residence time of the reaction products in the reactor.

[0064] S150, in response to determining that it is the activity activation event or the rapid inactivation event, the frequency of acquiring the composition data is increased.

[0065] To better understand the automated control method proposed in this application, some key terms and implementation environments involved are explained below.

[0066] This method is mainly applied to gas-solid phase catalytic reaction processes, which are typically carried out in a reactor containing a catalyst bed. The feed gas reacts through the catalyst bed, transforming into reaction products.

[0067] "Composition data" refers to the information on the types and contents of each component in the reaction products at the reactor outlet, which is usually obtained through online analytical instruments.

[0068] "Activity index" is a parameter that measures the catalytic performance of a catalyst, such as feed gas conversion rate or target product selectivity.

[0069] "Smoothing" refers to filtering the raw activity index data to eliminate noise and short-term fluctuations, making its trend clearer.

[0070] "Rate of change" refers to the rate at which the activity index changes with time or temperature, reflecting the dynamic trend of catalyst activity.

[0071] "Excitation threshold" and "deactivation threshold" are preset criteria used to identify events in which the activity of the catalyst changes significantly.

[0072] The "heating stage" refers to the process by which the reactor is heated according to a preset temperature-time curve.

[0073] The "constant temperature operation stage" refers to the stage in which the reactor operates stably at a set temperature.

[0074] "Average residence time" refers to the average length of time that reactants remain in the reactor, and it is closely related to the feed gas flow rate.

[0075] "Sampling frequency" refers to the rate at which data on the composition of the reaction products are sampled.

[0076] First, the composition data of the reaction products at the reactor outlet is acquired in real time, and the catalyst activity indicators are obtained based on this data. The composition data can be acquired in various ways. For example, offline analysis methods can be used, periodically sampling from the reactor outlet and then sending the samples to a laboratory for gas chromatography analysis to obtain the concentration of each component. Another approach is to install an online analyzer at the reactor outlet, such as an online mass spectrometer or Fourier transform infrared spectrometer. These instruments can monitor the concentration changes of specific components in the reaction products in real time. Based on this composition data, various activity indicators can be calculated. For example, the feed gas conversion rate can be obtained by calculating the ratio of the consumption of a specific feed gas to the initial feed rate. Alternatively, product selectivity can be obtained by calculating the ratio of the amount of the target product generated to the total amount of all products generated. These indicators can intuitively reflect the catalytic performance of the catalyst.

[0077] Secondly, the activity index is smoothed, and the rate of change of the processed activity index is calculated periodically. The raw data of the activity index often contains noise, and directly calculating the rate of change may be affected by interference. Therefore, smoothing is necessary. For example, a simple moving average method can be used, where the average of the activity index at the current moment and several previous moments is taken as the smoothed value for the current moment. Another approach is to use exponential smoothing, assigning different weights to historical data for a weighted average. After smoothing, the rate of change of the activity index needs to be calculated periodically. For example, the change in the activity index within a fixed time interval (e.g., 1 minute, 5 minutes) can be calculated, and the result divided by the time interval to obtain the rate of change. Alternatively, when the reactor temperature changes, the change in the activity index at a fixed temperature change (e.g., 1°C, 5°C) can be calculated, and the result divided by the temperature change to obtain the rate of change.

[0078] During the heating phase of the reactor, which is being heated according to a preset temperature-time curve, if the rate of change exceeds a preset activation threshold, an activation event is triggered. The heating phase is then paused, and the reactor temperature is locked at the temperature at which the activation event was detected, and maintained at this temperature for a preset isothermal duration. After the isothermal duration ends, the paused heating phase resumes from the detected temperature. During the catalyst activation process, a sudden and significant increase in activity may occur, i.e., activation. If the system continues heating according to the preset curve, it may miss the optimal activation temperature, resulting in insufficient or over-activation of the catalyst. When the rate of change of the activity index exceeds the preset activation threshold, it indicates that the catalyst activity is rapidly increasing, and the system immediately pauses the current heating program. For example, the heating unit can be stopped or its current heating power maintained to stabilize the reactor temperature at the temperature at which the activation event was detected. Subsequently, the system maintains this temperature at a preset isothermal duration to ensure that the catalyst is fully activated at this optimal temperature. After the constant temperature period ends, the system will resume the previously paused heating phase from that temperature point to complete the subsequent heating process.

[0079] During the isothermal operation of the reactor, when the rate of change is less than a preset deactivation threshold, a rapid deactivation event is triggered, and the flow rate of the feed gas is increased to shorten the average residence time of the reaction products in the reactor. During the isothermal operation of the catalytic reaction, catalyst activity may decrease due to various reasons, such as carbon buildup, poisoning, or sintering. When the rate of change of the activity index is lower than the preset deactivation threshold, it indicates that the catalyst is rapidly deactivating. To slow down the deactivation process or assess the cause of deactivation, the system will take intervention measures. For example, the flow rate of the feed gas can be increased by increasing the set value of the gas mass flow controller on the inlet pipeline. The increase in feed gas flow shortens the average residence time of the reactants in the reactor, which helps reduce the occurrence of side reactions or, to some extent, "washes away" some of the deactivated substances on the catalyst surface, thereby temporarily improving apparent activity.

[0080] In response to the determination of an activation event or a rapid deactivation event, the frequency of composition data acquisition is increased. When an activation event or rapid deactivation event occurs, it signifies a significant change in catalyst performance, requiring more intensive data to capture these dynamic processes. For example, during normal operation, the composition data acquisition frequency might be set to once every 5 minutes. When an activation event is triggered, the system can automatically increase the acquisition frequency to once every 1 minute or even higher to more precisely record the entire process of activity enhancement. Similarly, when a rapid deactivation event is triggered, increasing the acquisition frequency helps to more accurately monitor the rate and pattern of deactivation, providing more detailed data support for subsequent diagnosis and treatment. This mechanism of dynamically adjusting the acquisition frequency ensures that sufficient data is acquired at critical moments, avoiding the omission of important information.

[0081] The automated control method for catalytic reaction analysis instruments proposed in this application intelligently identifies and locks onto the "activation point" of a sudden increase in catalyst activity during the programmed temperature rise phase, conducting isothermal observation to accurately capture the optimal activation temperature. This avoids the defects of fixed temperature rise programs, which may miss the activation window or lead to insufficient activation. During the isothermal operation phase, when rapid deactivation is detected, the system can automatically adjust operating parameters (such as shortening the residence time) to attempt intervention and provide real-time diagnostic clues for the root cause of deactivation based on the catalyst's response pattern, realizing a shift from passive recording to proactive analysis and diagnosis. When the reaction characteristics of the catalyst under test are unclear or long-term stability assessment is required, the system can respond in real time and autonomously adjust experimental strategies. In addition, the system automatically increases the data acquisition frequency during critical event triggering, performs in-depth analysis and identification of performance change patterns, ensures high resolution and completeness of data during periods of drastic performance changes, and reduces the probability of experimental failure or misjudgment of the true performance of the catalyst.

[0082] In summary, this application, by introducing mechanisms such as real-time activity index monitoring, dynamic temperature locking, flow rate adjustment, and adaptive data acquisition frequency adjustment, enables catalytic reaction analysis instruments to more intelligently and flexibly cope with the complex behavior of catalysts, improving the adaptability of experiments, the effectiveness of data acquisition, and the accuracy of result judgment, and providing strong technical support for the development and application of novel catalysts.

[0083] In some embodiments of this application, the step of acquiring the composition data of the reaction products at the reactor outlet in real time, and acquiring the catalyst activity index based on the composition data, preferably includes:

[0084] The concentrations of each component of the reaction product at the reactor outlet are obtained using an online gas chromatograph installed in the reactor.

[0085] Based on the concentration of each component of the reaction products, the feed gas conversion rate or product selectivity is calculated as an indicator of catalyst activity.

[0086] Online gas chromatographs (GCs) are widely used instruments in chemical analysis, configured to separate, detect, and quantitatively analyze the components in gas mixtures. By placing the online GC directly at the reactor outlet, continuous and automated monitoring of the gaseous components of the reaction products can be achieved. This allows for real-time acquisition of the concentration data of each component in the reaction products; for example, the precise concentrations of target products, byproducts, and unconverted feed gas can be obtained. The concentrations of each component are typically expressed as mole fraction, volume percentage, or mass percentage, providing detailed information on the distribution of substances in the reaction system.

[0087] After obtaining the concentration data of each component of the reaction products, the catalyst's activity index can be calculated. This activity index can be specifically defined as feed gas conversion rate or product selectivity. Feed gas conversion rate refers to the proportion of a specific feed gas component converted into reaction products during the catalytic reaction, directly reflecting the catalyst's ability to consume feed gas. For example, for the reaction A→B, the conversion rate can be expressed as (initial moles of A - outlet moles of A) / initial moles of A. Product selectivity refers to the proportion of the target product among all products that may be generated, reflecting the catalyst's preference for generating a specific product. For example, for the reactions A→B and A→C, the selectivity of B can be expressed as moles of B / (moles of B + moles of C). These indicators can directly and quantitatively evaluate the catalyst's performance under specific reaction conditions.

[0088] This application's solution utilizes an online gas chromatograph to achieve real-time and accurate acquisition of the reactor outlet reaction product composition data. The online gas chromatograph can continuously analyze gas samples, providing real-time data on the concentration of each component, thus providing a reliable basis for subsequent activity index calculations. Based on this real-time component concentration data, the catalyst's activity state can be directly and quantitatively reflected by calculating the feed gas conversion rate or product selectivity. This method avoids the lag of manual sampling and offline analysis, ensuring the real-time nature and accuracy of activity indexes, and providing timely and effective data support for subsequent automated control decisions.

[0089] Based on the above embodiments, the step of smoothing the activity index and periodically calculating the rate of change of the processed activity index preferably includes:

[0090] The activity index is smoothed and filtered in real time using a moving average filtering algorithm.

[0091] Based on the processed activity index, the change in the activity index per unit time is calculated according to a preset time period, or the change in the activity index per unit temperature change is calculated according to a preset temperature change interval.

[0092] The change is taken as the rate of change of the activity index after processing.

[0093] In order to effectively eliminate random noise and instantaneous fluctuations in the data after acquiring the catalyst activity index in real time, thereby improving the reliability and stability of the activity index, a moving average filtering algorithm can be used to perform real-time smoothing filtering on the activity index. The moving average filtering algorithm smooths the data by calculating the average value of the data within a certain time window, which can effectively filter out high-frequency noise, making the trend of the activity index clearer and providing a more stable data foundation for subsequent analysis.

[0094] The method for calculating the rate of change of the treated activity index can be flexibly selected according to actual needs and reaction characteristics. A preferred implementation is to calculate the change in the activity index per unit time period based on the treated activity index, such as calculating the increase or decrease in the activity index every minute or five minutes. Another preferred implementation is to calculate the change in the activity index per unit temperature change interval based on the treated activity index, such as the change in the activity index when the temperature increases or decreases by one degree Celsius. Both calculation methods aim to quantify the rate of change of the activity index with time or temperature, facilitating accurate subsequent judgment of the catalyst state. In practical applications, the calculated change is directly used as the rate of change of the treated activity index, which directly reflects whether the catalyst activity is increasing, decreasing, or remaining stable.

[0095] This application's solution effectively addresses the potential noise interference in the original activity index data by introducing a moving average filtering algorithm, ensuring the accuracy of subsequent rate-of-change calculations. By periodically calculating the rate of change of the smoothed activity index, whether based on a time period or temperature change interval, a quantitative indicator can be provided to monitor the dynamic changes in catalyst activity in real time. This dynamic monitoring mechanism enables the system to promptly capture early signs of activity activation or rapid deactivation, providing a reliable data foundation for subsequent automated control decisions. For example, during the heating phase, monitoring the rate of change of the activity index can accurately identify the temperature point at which catalyst activity is activated; during the isothermal operation phase, it can promptly detect the rapid deactivation trend of the catalyst.

[0096] In a specific embodiment of this application, the step of determining that an activation event is triggered when the rate of change of the reactor during the heating phase according to a preset temperature-time curve exceeds a preset activation threshold, pausing the heating phase, locking the reactor temperature at the temperature point at which the activation event was detected, and maintaining the temperature for a preset isothermal duration; and resuming the suspended heating phase from the temperature point after the isothermal duration has ended preferably includes:

[0097] When the reactor is in the heating phase according to a preset temperature-time curve, an activation event is determined when the rate of change exceeds a preset activation threshold. The activation threshold is positive, meaning that an activation event is only identified when the catalyst's activity index shows a clear and continuous upward trend. This helps eliminate misjudgments caused by measurement noise or instantaneous fluctuations, ensuring that the determined activation events are genuine and valid.

[0098] In response to the activation event, the temperature point at which the activation event is detected is recorded. Recording the temperature point means accurately saving the real-time temperature value inside the reactor at the time the activation event is triggered. This temperature point is a critical reference point for subsequent temperature locking and curve recovery, and its accurate recording is essential to ensuring the accuracy of control.

[0099] The ongoing temperature-time curve is modified by adding a constant-temperature segment, starting from the time corresponding to the temperature point. The temperature of this segment is the detected temperature point, and its duration is a preset constant-temperature duration. This pauses the heating phase and locks the reactor temperature. This operation is not simply stopping heating, but rather dynamically modifying the preset temperature-time curve to insert a constant-temperature segment with a specific temperature and duration at the detected temperature point. The temperature of this constant-temperature segment is precisely set to the detected temperature point, and its duration is determined by the preset constant-temperature duration. In this way, the reactor can smoothly transition from a heating state to a constant-temperature state and precisely lock the temperature at the point of activation, thus providing stable conditions for the full activation of the catalyst.

[0100] After the isothermal phase ends, the reactor is controlled to resume execution from the temperature point, resuming the portion of the temperature-time curve that follows the isothermal phase, thus resuming the paused heating stage. Resuming execution means that after the preset isothermal duration, the control system continues heating according to the portion of the original temperature-time curve that follows the isothermal phase. This recovery mechanism ensures the continuity and integrity of the experimental process, avoiding experimental interruptions or deviations in the temperature curve caused by handling activation events.

[0101] Through the above technical solution, this application can significantly improve the accuracy and reliability of determining catalyst activity activation events, avoiding experimental interruptions or unnecessary temperature adjustments due to misjudgments. Furthermore, by precisely recording temperature points and dynamically adjusting the temperature-time curve, stable locking and seamless recovery of the reactor temperature are achieved, ensuring that the catalyst can be stably maintained at the optimal temperature during activation, thereby optimizing the catalyst activation effect and improving the stability and reproducibility of experimental results. This refined temperature control strategy contributes to a deeper understanding of the catalyst activation mechanism and provides a more reliable foundation for subsequent catalytic reaction research.

[0102] The following will illustrate this with specific examples.

[0103] Suppose that during the heating process, the conversion rate (as an activity indicator) of a catalyst begins to rise rapidly at 300℃. At this point, the system calculates the rate of change of the activity indicator in real time to be 0.5% / min, while the preset activation threshold is 0.2% / min (a positive value). Since 0.5% is greater than 0.2%, the system determines that an activity activation event has been triggered. The system then precisely records the current reactor temperature as 300℃. To pause the heating and lock the temperature, the control system modifies the original temperature-time curve, inserting a 30-minute isothermal interval at 300℃. During these 30 minutes, the reactor temperature is precisely maintained at 300℃, allowing the catalyst to be fully activated. After the 30-minute isothermal period, the control system resumes the portion of the original temperature-time curve after 300℃, for example, continuing to heat to 400℃ at a rate of 5℃ / min, thus ensuring the continuity of the entire experimental process and the preset temperature program.

[0104] In a more specific embodiment of this application, the temperature-time curve, starting from the time corresponding to the temperature point, adds a constant-temperature segment, the temperature of which is the temperature point, and the duration of which is the preset constant-temperature duration, preferably including the step of pausing the heating phase and locking the reactor temperature as follows:

[0105] The temperature-time curve currently being executed will be extended to include a constant temperature segment starting from the time corresponding to the temperature point, and an internal thermal management operation synchronized with the constant temperature segment will be initiated. The temperature of the constant temperature segment is the temperature point, and the duration of the constant temperature segment is the preset constant temperature duration.

[0106] The internal thermal management operation includes pre-cooling the feed gas, injecting inert gas into the feed gas, and starting a thermosiphon cycle to drive the inert gas to circulate within the catalyst bed to homogenize the temperature.

[0107] It should be noted that the internal thermal management operations refer to a series of auxiliary measures taken during the isothermal phase, when the reactor temperature is locked, to ensure the stability and uniformity of the internal environment of the catalyst bed. Pre-cooling the feed gas aims to reduce its temperature upon entering the reactor, preventing localized thermal shock to the catalyst bed or the initiation of undesirable reactions due to excessively high feed gas temperature during the isothermal phase. Injecting an inert gas, such as nitrogen or helium, into the feed gas dilutes the reactant concentration in the catalyst bed, reduces or suppresses potential side reactions during the isothermal phase, and serves as a carrier gas to assist in heat transfer. Activating a thermosiphon circulation to drive the inert gas to circulate within the catalyst bed to homogenize the temperature involves utilizing the fluid density changes caused by temperature differences to create natural circulation of the inert gas within the catalyst bed. This effectively transfers heat from high-temperature regions to low-temperature regions, ensuring that the entire catalyst bed achieves and maintains a highly uniform temperature distribution during the isothermal phase.

[0108] By employing the above technical solution, when an activity activation event is detected and the reactor temperature is locked, the temperature uniformity within the catalyst bed and the stability of the reaction environment can be ensured. Compared to a basic solution that only locks the temperature, this application, by introducing internal thermal management operations, effectively avoids potential localized overheating, temperature gradients, and undesirable side reactions within the catalyst bed. This improves the accuracy of activity activation event detection and ensures the effectiveness and controllability of the catalyst activation process. Therefore, the solution of this application can more precisely control the catalyst's activation state, optimize catalytic reaction performance, and extend the catalyst's lifespan.

[0109] In a further embodiment of this application, the step of determining that a rapid deactivation event is triggered and increasing the flow rate of the raw material gas to shorten the average residence time of the reaction products in the reactor when the reactor is in a constant temperature operation phase and the rate of change is less than a preset deactivation threshold preferably includes:

[0110] When the reactor is in a constant temperature operation phase, if the rate of change is less than a preset deactivation threshold, it is determined to be a rapid deactivation event; wherein, the deactivation threshold is negative.

[0111] In response to the rapid deactivation event, the set value of the gas mass flow controller installed on the inlet line of the reactor is increased to increase the flow rate of the feed gas, thereby reducing the average residence time of the reactants in the reactor by a preset adjustment ratio.

[0112] After changing the average residence time and maintaining the preset observation duration, the rate of change of the activity index is recalculated, and the inactive substance is judged.

[0113] It should be noted that during the isothermal operation of the reactor, the system continuously monitors the rate of change of catalyst activity indicators. When this rate of change is less than a preset deactivation threshold, a rapid deactivation event is identified as triggered. This deactivation threshold is set to a negative value because a decrease in catalyst activity typically manifests as a reduction in activity indicators, resulting in a negative rate of change. Therefore, setting the deactivation threshold to a negative value allows for precise definition of the critical state of rapid activity decline, ensuring that subsequent response mechanisms are triggered only when the rate of activity decline reaches a warning level.

[0114] In response to a rapidly deactivating event, the system increases the setpoint of the gas mass flow controller located on the reactor's inlet line. This increases the flow rate of the feed gas, effectively reducing the average residence time of the reactants in the reactor by a preset adjustment ratio. Shortening the average residence time aims to reduce the contact time between the reactants and the catalyst, thereby inhibiting or delaying further catalyst deactivation to some extent. Alternatively, by increasing the velocity of the reactants through the catalyst bed, impurities or byproducts that may lead to deactivation can be carried away from the catalyst surface more quickly, in order to restore or stabilize catalyst activity.

[0115] After adjusting the average residence time and maintaining operation for a preset observation period, the system recalculates the rate of change of catalyst activity indicators and uses this to determine the deactivated substance. This step aims to evaluate the effectiveness of the aforementioned flow rate adjustment measures and attempt to diagnose the root cause of rapid deactivation. By observing the rate of change of activity indicators after adjustment, it is possible to preliminarily infer whether deactivation is caused by excessive residence time, product inhibition, impurity poisoning, or other factors, providing crucial information for subsequent deeper diagnosis and intervention.

[0116] This application's solution, by introducing a negative deactivation threshold, can more accurately identify the critical state of rapid catalyst activity decline, avoiding insensitivity or misjudgment of activity decline. When a rapid activity decline is detected, increasing the feed gas flow rate can effectively shorten the average residence time of reactants in the catalyst bed. The principle behind this operation is that reducing the contact time between reactants and catalyst can reduce the risk of side reactions or carbon deposition on the catalyst surface, thereby inhibiting the deactivation process to some extent. In addition, increasing the flow rate also helps to quickly remove harmful substances or reaction byproducts adsorbed on the catalyst surface, thus creating conditions for the catalyst to recover some activity. More importantly, after taking initial flow rate adjustment measures, by maintaining the preset observation period and recalculating the rate of change of activity indicators, a preliminary judgment on the nature of deactivation can be made. For example, if the rate of activity decline slows down or stops after flow rate adjustment, it may indicate that deactivation is related to excessive residence time or product inhibition; if the trend of activity decline is still obvious, it may suggest the existence of a deeper deactivation mechanism, such as impurity poisoning or structural damage, thus providing key information for subsequent diagnosis and intervention.

[0117] The following is a specific example to illustrate this.

[0118] In a gas-solid phase catalytic reaction, the reactor operates at an isothermal temperature. The system continuously monitors the rate of change of catalyst activity indicators (e.g., feed gas conversion rate). When the rate of change of the activity indicator decreases from -0.01% / min to -0.05% / min, while the preset deactivation threshold is -0.03% / min, the system determines that a rapid deactivation event has been triggered because -0.05% / min is less than -0.03% / min. In response to this event, the system automatically increases the setpoint of the gas mass flow controller on the inlet line, for example, increasing the feed gas flow rate from 100 mL / min to 120 mL / min, thereby reducing the average residence time of the reactants in the reactor by 20%. After maintaining this new flow rate for 30 minutes, the system recalculates the rate of change of the activity indicator. If the rate of change rises back to -0.02% / min, it is preliminarily determined that the current deactivation may be related to excessive residence time or product inhibition. The system may continue to operate at the current flow rate and observe further. If the rate of change is still below -0.03% / min, for example -0.04% / min, it may indicate that there are other more serious causes of inactivation. The system may further trigger diagnostic procedures, such as switching the feed gas source or performing other more in-depth analyses to determine the fundamental nature of the inactivation.

[0119] In a further embodiment of this application, the step of recalculating the rate of change of the activity index and judging the inactive substance after changing the average residence time and maintaining the preset observation duration preferably includes:

[0120] After changing the average dwell time while maintaining the preset observation duration, the rate of change is recalculated;

[0121] If the recalculated rate of change is greater than or equal to the inactivation threshold after shortening the average residence time, it is preliminarily determined that the current inactivation has a tendency to be poisoned by impurities.

[0122] Based on the initial assessment that the current inactivation has a tendency to be poisoned by impurities, the current raw material gas source is switched to a backup high-purity raw material gas source, and the rate of change is monitored after the switch.

[0123] If the rate of change monitored after switching is greater than the preset attenuation threshold, then the rapid deactivation event is ultimately determined to be caused by impurities in the raw gas; wherein the attenuation threshold is negative and greater than the deactivation threshold.

[0124] In the event of rapid catalyst deactivation, the system first adjusts the feed gas flow rate according to the above-described procedure to shorten the average residence time of the reaction products in the reactor. After this operation and a preset observation period, the rate of change of the catalyst activity index is recalculated. This step aims to evaluate the effect of the initial adjustment, i.e., to determine whether shortening the residence time is sufficient to alleviate the deactivation phenomenon. The observation period can be set according to the response rate of the reaction system and the data acquisition frequency, for example, it can be set to several minutes to several hours to ensure that there is sufficient time for the system to reach a new quasi-steady state and obtain reliable activity data after the adjustment.

[0125] If the recalculated rate of change remains greater than or equal to the deactivation threshold after shortening the average residence time, it means that even with adjustments to the residence time, the catalyst's activity decline trend remains significant or has not been effectively improved. In this case, the system will initially determine that the current deactivation has a tendency to be poisoned by impurities. The deactivation threshold is negative, indicating a decrease in activity. When the recalculated rate of change is greater than or equal to this negative value, it indicates that the rate of activity decline is still rapid or has not slowed down significantly, which is consistent with the irreversible or difficult-to-reverse deactivation characteristics caused by impurity poisoning.

[0126] Based on the initial assessment that the current deactivation shows a tendency towards impurity poisoning, the system will take further intervention measures, namely switching the currently used feed gas source to a backup high-purity feed gas source. This operation aims to eliminate the continued poisoning effect of any impurities in the feed gas on the catalyst. After the gas source switch is completed, the system will continuously monitor the rate of change of catalyst activity indicators to assess the impact of the high-purity feed gas on the activator activity.

[0127] If the monitored rate of change after switching exceeds a preset attenuation threshold, the rapid deactivation event is ultimately determined to be caused by impurities in the feed gas. The attenuation threshold is negative and greater than the deactivation threshold, meaning that the attenuation threshold represents a less severe rate of activity decline than the deactivation threshold (e.g., the deactivation threshold might be -0.5% / min, while the attenuation threshold might be -0.1% / min). If, after switching to a high-purity gas source, the rate of activity decline significantly slows down, or even stabilizes or slightly recovers, resulting in a rate of change greater than the attenuation threshold, it strongly suggests that impurities in the feed gas are the primary cause of rapid deactivation.

[0128] The proposed solution involves diagnosing the cause of catalyst deactivation after initial adjustment of the residence time, particularly verifying the possibility of impurity poisoning. By comparing the rate of activity change before and after adjustment, as well as before and after switching gas sources, the system can gradually eliminate other deactivation factors and ultimately confirm whether it is caused by impurities in the feed gas. This step-by-step diagnostic and verification mechanism allows the system to move beyond simple kinetic adjustments to a deeper understanding of the nature of deactivation, enabling more targeted interventions.

[0129] The following is a specific example to illustrate this.

[0130] Assuming that during the isothermal operation phase of the catalytic reaction, the system detects a rate of change of -0.6% / min for the catalyst's activity index, which is less than the preset deactivation threshold of -0.5% / min, thus triggering a rapid deactivation event. The system then increases the feed gas flow rate, shortens the average residence time of the reaction products in the reactor by 20%, and maintains this for a 30-minute observation period. After 30 minutes, the system recalculates the rate of change of the activity index and finds it remains at -0.4% / min. Although slightly improved, this value is still greater than or equal to the deactivation threshold of -0.5% / min, indicating that simply shortening the residence time has not effectively solved the problem. Therefore, it is initially determined that the current deactivation has a tendency to be caused by impurity poisoning. Based on this initial judgment, the system automatically switches the current feed gas source to a backup high-purity feed gas source. After the switch, the system continues to monitor the rate of change of the activity index. Within 15 minutes after the switch, the monitored rate of change gradually recovers to -0.05% / min. Since this value is greater than the preset decay threshold of -0.1% / min, the system ultimately determines that this rapid deactivation event is caused by impurities in the feed gas. Through this series of diagnoses and interventions, the system can promptly detect and resolve issues related to impurities in the raw material gas, preventing further poisoning of the catalyst and ensuring the smooth progress of the experiment.

[0131] In some embodiments of this application, the step of increasing the frequency of compositional data acquisition in response to a determination of an activation event or a rapid inactivation event preferably includes:

[0132] In response to whether an event is determined to be an activation event or a rapid inactivation event, the absolute difference between the rate of change and the activation threshold or inactivation threshold is calculated.

[0133] Based on the absolute difference, a frequency increase value is determined, and the frequency increase value is positively correlated with the absolute difference.

[0134] The improved sampling frequency is obtained by adding the initial sampling frequency to the constituent data.

[0135] When the system determines that an activity activation event or a rapid inactivation event has been triggered, it first needs to calculate the absolute difference between the rate of change of the currently detected activity index and the preset activation or inactivation threshold. This absolute difference can be understood as the "severity" or "deviation" of the event, that is, the extent to which the current rate of activity change deviates from the normal or expected threshold. For example, when the rate of change far exceeds the activation threshold, the absolute difference is large, indicating that the activity activation is very intense; when the rate of change is far below the inactivation threshold, the absolute difference is large, indicating that the rapid inactivation is very severe.

[0136] Based on the calculated absolute difference, a frequency increase value can be determined. There is a positive correlation between this frequency increase value and the absolute difference value, meaning that the more severe the event (the larger the absolute difference), the higher the required sampling frequency needs to be, and vice versa. This positive correlation can be achieved through a preset functional relationship, a lookup table, or a scaling factor. For example, a linear relationship can be set, where the frequency increase value equals the absolute difference multiplied by a scaling factor, or a piecewise function can be used, employing different increase strategies within different absolute difference intervals.

[0137] The increased sampling frequency is obtained by adding the initial sampling frequency of the constituent data to the determined frequency enhancement value. This means that when an event occurs, the system can dynamically adjust the density of data collection according to the severity of the event, thereby obtaining more detailed and timely data on the composition of the reaction products at critical moments.

[0138] This application's solution achieves adaptive adjustment of the composition data acquisition frequency by introducing the calculation of the absolute difference between the rate of change and a threshold, and positively correlated the frequency increase value with this absolute difference. When the catalyst activity undergoes drastic changes (whether rapid activation or rapid deactivation), the rate of change of the activity index will significantly deviate from the preset threshold, resulting in a large calculated absolute difference. Based on this large absolute difference, the system determines a higher frequency increase value, thereby significantly increasing the acquisition frequency of composition data. This mechanism ensures that when abnormal or critical changes occur in the catalytic reaction process, reaction product composition data can be acquired with higher resolution and faster speed, providing richer and more accurate real-time information for subsequent event analysis, diagnosis, and control.

[0139] The following is a specific example to illustrate this.

[0140] Assume that during the reactor's heating phase, the system detects a catalyst activity rate of 0.05% / s, while the preset activation threshold is 0.01% / s. The calculated absolute difference between this rate of change and the activation threshold is |0.05 - 0.01| = 0.04% / s. If there is a linear relationship between the preset frequency increase and the absolute difference, for example, frequency increase = absolute difference * 10 (unit: Hz / (% / s)), then the frequency increase will be determined as 0.04 * 10 = 0.4 Hz. If the initial data acquisition frequency is 0.1 Hz, the increased acquisition frequency will become 0.1 + 0.4 = 0.5 Hz.

[0141] For another example, when the reactor is in a constant-temperature operation phase, and the system detects a change rate of -0.08% / s for the activity index, while the preset inactivation threshold is -0.02% / s, the calculated absolute difference between the change rate and the inactivation threshold is |-0.08 - (-0.02)| = |-0.06| = 0.06% / s. Based on the same linear relationship, the frequency increase will be determined to be 0.06 * 10 = 0.6 Hz. If the initial sampling frequency is still 0.1 Hz, the increased sampling frequency will become 0.1 + 0.6 = 0.7 Hz.

[0142] As can be seen from the above examples, the more drastic the change in activity (i.e., the larger the absolute difference), the greater the increase in the sampling frequency. This ensures that more dense and detailed reaction product composition data can be obtained at critical moments to support more accurate analysis and control.

[0143] In a further embodiment of this application, the step of increasing the frequency of acquiring the composition data in response to the determination of the activity activation event or the rapid inactivation event preferably further includes the following step:

[0144] Generate a record containing the timestamp of the activation event or the rapid deactivation event, the event type, the rate of change, and the relevant parameters and values ​​before and after the temperature lock, dwell time adjustment and acquisition frequency adjustment operations performed;

[0145] The records are stored in the reactor's experimental log for traceability.

[0146] It should be noted that "record generation" refers to the automatic creation of a structured data entry after the system detects an activation event or rapid deactivation event and executes the corresponding control operation. This data entry contains the exact time point of the event, i.e., a timestamp. The event type clearly indicates whether it is an activation event or a rapid deactivation event. Furthermore, the record also includes the specific numerical value of the rate of change of the activity index when the event is triggered, as well as detailed parameters of the various operations performed by the system in response to this event. Examples include the temperature point locked and the isothermal duration for temperature locking operations, the percentage increase in feed gas flow rate or reduction in average residence time for residence time adjustment operations, and the acquisition frequency values ​​before and after acquisition frequency adjustment operations. The recording of these parameters and values ​​aims to comprehensively reflect the system state and the response behavior of the control system at the time of the event. Storing these records in the reactor's experimental log can be understood as persistently saving the generated data entry. The experimental log can be a database, a text file, or any other medium suitable for storing structured data. Its purpose is to ensure that this critical information is not lost and can be easily retrieved and consulted during subsequent analysis, troubleshooting, or experimental reproduction. In this way, the entire automated control process can be effectively traced, providing valuable data support for researchers and engineers.

[0147] The following will illustrate this with specific examples.

[0148] Suppose that during the heating phase of a catalytic reaction, the system detects a sudden increase in the rate of change of the catalyst's activity index, exceeding a preset activation threshold, thus triggering an activity activation event. At this point, the system immediately pauses the heating, locking the reactor temperature at the point where the event was detected and maintaining this temperature for a preset duration. Simultaneously, the system increases the frequency of data acquisition for the reaction product composition. While performing these control operations, the system automatically generates a record containing: a timestamp (e.g., 2023-10-27 10:35:12), event type (activity activation event), rate of change (e.g., +0.05% / min), the temperature locking operation performed (locked temperature 250℃, isothermal duration 30 min), and the data acquisition frequency adjustment operation (previously 1 time / min, now 5 times / min). This record is then stored in the reactor's experimental log.

[0149] For example, during another isothermal operation, the system detected a continuous decrease in the rate of change of the catalyst's activity index, falling below the preset deactivation threshold, thus triggering a rapid deactivation event. The system immediately increases the feed gas flow rate to shorten the average residence time of the reaction products in the reactor and increases the frequency of composition data acquisition. Similarly, the system generates a record containing a timestamp (e.g., 2023-10-28 14:20:05), event type (rapid deactivation event), rate of change (e.g., -0.02% / min), the residence time adjustment operation performed (feed gas flow rate increased from 100 ml / min to 120 ml / min, average residence time reduced by 20%), and the acquisition frequency adjustment operation (frequency 1 time / min before adjustment, frequency 5 times / min after adjustment). This record is also stored in the experimental log. By reviewing these experimental logs, researchers can clearly understand the trend of catalyst activity changes throughout the experiment, when and how the system responds to these changes, and the impact of these responses on subsequent reaction processes. This has important guiding significance for analyzing the performance degradation mechanism of catalysts, optimizing reaction conditions, and improving automated control algorithms.

[0150] like Figure 2 As shown, this application also discloses an automated control system 200 for a catalytic reaction analysis instrument, used to control a gas-solid phase catalytic reaction process, wherein the gas-solid phase catalytic reaction process includes converting the feed gas into reaction products by passing it through a reactor containing a catalyst bed, and the system includes:

[0151] The index acquisition module 210 is used to acquire the composition data of the reaction products at the reactor outlet in real time, and to acquire the activity index of the catalyst based on the composition data.

[0152] The speed calculation module 220 is used to smooth the activity index and periodically calculate the rate of change of the processed activity index.

[0153] The heating control module 230 is used to determine that an activation event is triggered when the rate of change of the reactor is greater than a preset activation threshold during the heating phase of heating according to a preset temperature-time curve, pause the heating phase, lock the temperature of the reactor at the temperature point at which the activation event is detected, and maintain the temperature for a preset constant time; after the constant temperature time ends, the paused heating phase is resumed starting from the temperature point.

[0154] The constant temperature control module 240 is used to determine that a rapid deactivation event is triggered when the rate of change is less than a preset deactivation threshold during the constant temperature operation phase of the reactor, thereby increasing the flow rate of the raw material gas to shorten the average residence time of the reaction products in the reactor.

[0155] The frequency adjustment module 250 is used to increase the acquisition frequency of the component data in response to the determination of the active activation event or the rapid deactivation event.

[0156] Specifically, the indicator acquisition module 210 can be configured to communicate with an online analytical instrument (e.g., an online gas chromatograph, mass spectrometer, or Fourier transform infrared spectrometer) at the reactor outlet to receive composition data of the reaction products in real time.

[0157] The speed calculation module 220 can be implemented as a software algorithm unit and run on the system's central processing unit.

[0158] The heating control module 230 can be designed as a hardware-software co-module that integrates a temperature sensor, a heating controller, and a logic judgment unit.

[0159] The temperature control module 240 can be configured to work in conjunction with the gas mass flow controller and the logic decision unit.

[0160] The frequency adjustment module 250 can be implemented as a data acquisition and control unit, which is connected to the data acquisition hardware of the indicator acquisition module.

[0161] It should be noted that the information interaction and execution process between the above modules are based on the same concept as the method embodiments of this application. For details on their specific functions and technical effects, please refer to the method embodiments section, which will not be repeated here.

[0162] The foregoing has provided a detailed description of the preferred embodiments of this application. However, this application is not limited to the above-described embodiments. Those skilled in the art can make various equivalent modifications or substitutions without departing from the spirit of this application. All such equivalent modifications or substitutions are included within the scope defined in this application.

Claims

1. An automated control method for a catalytic reaction analysis instrument, characterized in that, A method for controlling a gas-solid phase catalytic reaction process, the gas-solid phase catalytic reaction process comprising converting a feed gas into reaction products by passing it through a reactor containing a catalyst bed, the method comprising the following steps: The composition data of the reaction products at the reactor outlet are acquired in real time, and the activity index of the catalyst is obtained based on the composition data. The activity index is smoothed, and the rate of change of the processed activity index is periodically calculated. When the reactor is in the heating phase according to a preset temperature-time curve, if the rate of change is greater than a preset activation threshold, an activation event is triggered, the heating phase is paused, the temperature of the reactor is locked at the temperature point at which the activation event was detected, and the temperature is maintained for a preset constant temperature duration; after the constant temperature duration ends, the paused heating phase is resumed starting from the temperature point. When the reactor is in the isothermal operation stage, if the rate of change is less than a preset deactivation threshold, a rapid deactivation event is triggered, and the flow rate of the raw material gas is increased to shorten the average residence time of the reaction products in the reactor. In response to the determination of the activity activation event or the rapid inactivation event, the frequency of acquiring the composition data is increased.

2. The automated control method for a catalytic reaction analysis instrument according to claim 1, characterized in that, The step of acquiring the composition data of the reaction products at the reactor outlet in real time, and obtaining the catalyst activity index based on the composition data, includes: The concentrations of each component of the reaction product at the reactor outlet are obtained using an online gas chromatograph installed in the reactor. Based on the concentration of each component of the reaction products, the feed gas conversion rate or product selectivity is calculated as an indicator of catalyst activity.

3. The automated control method for a catalytic reaction analysis instrument according to claim 1, characterized in that, The step of smoothing the activity index and periodically calculating the rate of change of the processed activity index includes: The activity index is smoothed and filtered in real time using a moving average filtering algorithm. Based on the processed activity index, the change in the activity index per unit time is calculated according to a preset time period, or the change in the activity index per unit temperature change is calculated according to a preset temperature change interval. The change is taken as the rate of change of the activity index after processing.

4. The automated control method for a catalytic reaction analysis instrument according to claim 1, characterized in that, When the reactor is in the heating phase according to a preset temperature-time curve, if the rate of change is greater than a preset activation threshold, an activation event is determined to be triggered, the heating phase is paused, the temperature of the reactor is locked at the temperature point at which the activation event was detected, and the preset constant temperature duration is maintained. After the isothermal period ends, the steps to resume the suspended heating phase from the temperature point include: When the reactor is in the heating phase according to a preset temperature-time curve, if the rate of change is greater than a preset activation threshold, it is determined to be an activation event; wherein, the activation threshold is positive. In response to the activity activation event, the temperature point at which the activity activation event is detected is recorded; The temperature-time curve being executed is extended by adding a constant temperature segment starting from the time corresponding to the temperature point. The temperature of the constant temperature segment is the temperature point, and the duration of the constant temperature segment is the preset constant temperature duration, so as to pause the heating phase and lock the temperature of the reactor. After the isothermal phase ends, the reactor is controlled to resume execution from the temperature point, resuming the portion of the temperature-time curve that follows the isothermal phase, in order to resume the suspended heating phase.

5. The automated control method for a catalytic reaction analysis instrument according to claim 4, characterized in that, The step of adding a constant-temperature segment to the currently executing temperature-time curve, starting from the time corresponding to the temperature point, wherein the temperature of the constant-temperature segment is the temperature point, and the duration of the constant-temperature segment is a preset constant-temperature duration, to pause the heating phase and lock the reactor temperature includes: The temperature-time curve currently being executed will be extended to include a constant temperature segment starting from the time corresponding to the temperature point, and an internal thermal management operation synchronized with the constant temperature segment will be initiated. The temperature of the constant temperature segment is the temperature point, and the duration of the constant temperature segment is the preset constant temperature duration. The internal thermal management operation includes pre-cooling the feed gas, injecting inert gas into the feed gas, and starting a thermosiphon cycle to drive the inert gas to circulate within the catalyst bed to homogenize the temperature.

6. The automated control method for a catalytic reaction analysis instrument according to claim 1, characterized in that, The step of determining that a rapid deactivation event is triggered when the rate of change is less than a preset deactivation threshold during the isothermal operation of the reactor, and increasing the flow rate of the feed gas to shorten the average residence time of the reaction products in the reactor, includes: When the reactor is in a constant temperature operation phase, if the rate of change is less than a preset deactivation threshold, it is determined to be a rapid deactivation event; wherein, the deactivation threshold is negative. In response to the rapid deactivation event, the set value of the gas mass flow controller installed on the inlet line of the reactor is increased to increase the flow rate of the feed gas, thereby reducing the average residence time of the reactants in the reactor by a preset adjustment ratio. After changing the average residence time and maintaining the preset observation duration, the rate of change of the activity index is recalculated, and the inactive substance is judged.

7. The automated control method for a catalytic reaction analysis instrument according to claim 6, characterized in that, The step of recalculating the rate of change of the activity index and judging the inactive substance after changing the average residence time and maintaining the preset observation duration includes: After changing the average dwell time while maintaining the preset observation duration, the rate of change is recalculated; If the recalculated rate of change is greater than or equal to the inactivation threshold after shortening the average residence time, it is preliminarily determined that the current inactivation has a tendency to be poisoned by impurities. Based on the initial assessment that the current inactivation has a tendency to be poisoned by impurities, the current raw material gas source is switched to a backup high-purity raw material gas source, and the rate of change is monitored after the switch. If the rate of change monitored after switching is greater than the preset attenuation threshold, then the rapid deactivation event is ultimately determined to be caused by impurities in the raw gas; wherein the attenuation threshold is negative and greater than the deactivation threshold.

8. The automated control method for a catalytic reaction analysis instrument according to claim 1, characterized in that, The step of increasing the acquisition frequency of the component data in response to the determination of the activity activation event or the rapid inactivation event includes: In response to the determination of the activity activation event or the rapid inactivation event, the absolute difference between the rate of change and the activation threshold or the inactivation threshold is calculated; Based on the absolute difference, a frequency increase value is determined, and the frequency increase value is positively correlated with the absolute difference. The improved sampling frequency is obtained by adding the initial sampling frequency to the constituent data.

9. The automated control method for a catalytic reaction analysis instrument according to claim 1, characterized in that, Following the step of increasing the acquisition frequency of the composition data in response to the determination of the activity activation event or the rapid inactivation event, the method further includes the following steps: Generate a record containing the timestamp of the activation event or the rapid deactivation event, the event type, the rate of change, and the relevant parameters and values ​​before and after the temperature lock, dwell time adjustment and acquisition frequency adjustment operations performed; The records are stored in the reactor's experimental log for traceability.

10. An automated control system for a catalytic reaction analysis instrument, characterized in that, For controlling a gas-solid phase catalytic reaction process, the gas-solid phase catalytic reaction process comprising converting a feed gas into reaction products through a reactor containing a catalyst bed, the system comprising: The index acquisition module is used to acquire the composition data of the reaction products at the reactor outlet in real time, and to acquire the activity index of the catalyst based on the composition data. The speed calculation module is used to smooth the activity index and periodically calculate the rate of change of the processed activity index. The heating control module is used to determine that an activation event is triggered when the rate of change of the reactor exceeds a preset activation threshold during the heating phase of heating according to a preset temperature-time curve. The heating phase is then paused, and the temperature of the reactor is locked at the temperature point at which the activation event was detected, and maintained for a preset constant temperature duration. After the constant temperature duration ends, the paused heating phase is resumed starting from the temperature point. The constant temperature control module is used to determine and trigger a rapid deactivation event when the rate of change is less than a preset deactivation threshold during the constant temperature operation phase of the reactor, thereby increasing the flow rate of the raw material gas to shorten the average residence time of the reaction products in the reactor. A frequency adjustment module is used to increase the acquisition frequency of the component data in response to the determination of the active activation event or the rapid inactivation event.

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