Air pre-impurity-removal control method and system for Kr enrichment and separation

Abstract

The invention relates to an air pre-impurity-removal control method and system for enrichment and separation of Kr, and relates to the technical field of gas separation and purification, and the air pre-impurity-removal control method comprises the following steps: removing impurity components in air through an impurity removal device to obtain air subjected to impurity removal treatment; carrying out multi-stage enrichment and separation treatment on the air subjected to impurity removal treatment to obtain enriched Kr gas; and introducing the enriched Kr gas into a chromatographic separation device, and separating krypton from other inert gases to obtain a target krypton component. The problems that in the traditional Kr enrichment and separation process, due to the fact that air impurities are prone to icing, the device is blocked, the multi-stage separation parameter adaptability is poor, and the enrichment efficiency is low are solved, and through pre-impurity removal of intelligent parameter configuration and multi-stage enrichment of gradient temperature control, the Kr separation stability, the enrichment efficiency and the target component purity are improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of gas separation and purification, in particular to an air pre-purification control method and system for Kr enrichment separation. BACKGROUND

[0002] With the development of industrial gas separation technology, as a kind of rare noble gas, krypton (Kr) is increasingly in demand in the fields of photoelectricity, nuclear industry, etc., and its efficient enrichment and separation has become a key technical problem. At present, the traditional Kr enrichment and separation method only relies on pre-purification fixed parameters, which is difficult to adapt to the dynamic changes of easy-to-freeze impurities, and is easy to cause low-temperature device blockage. At the same time, separation is carried out at a single temperature, which leads to incomplete adsorption of krypton and incomplete separation of other gases, affecting the separation efficiency and purity.

[0003] The existing processing method only removes impurities and separates by fixed operating parameters, without dynamically adjusting the device parameters in combination with the air attribute characteristics, resulting in unstable impurity removal effect, high loss rate of krypton during the separation process, which not only reduces the overall efficiency of Kr enrichment and separation, but also increases the equipment maintenance cost and energy consumption. SUMMARY

[0004] To solve the above technical problems, the present application provides an air pre-purification control method and system for Kr enrichment and separation, which improves the stability of Kr separation, avoids device blockage, enhances the adaptability of multi-stage separation parameters, improves the enrichment efficiency and target component purity, and optimizes the adaptability under different working conditions.

[0005] The embodiments of the present application disclose the following technical solutions: In a first aspect, the embodiments of the present application provide an air pre-purification control method for Kr enrichment and separation, which comprises: passing the air to be treated through a purification device to remove the easy-to-freeze impurity components in the air to be treated, and obtain purified air; performing multi-stage enrichment and separation treatment on the purified air to obtain enriched Kr gas; passing the enriched Kr gas into a chromatographic separation device to separate krypton and other inert gases, and obtain target krypton components.

[0006] In a second aspect, the embodiments of the present application provide an air pre-purification control system for Kr enrichment and separation, which comprises: an air pre-purification treatment module for passing the air to be treated through a purification device to remove the easy-to-freeze impurity components in the air to be treated, and obtain purified air; a multi-stage Kr enrichment and separation module for performing multi-stage enrichment and separation treatment on the purified air to obtain enriched Kr gas; The chromatographic separation and purification module is used for inputting the Kr-rich gas into a chromatographic separation device, separating krypton and other inert gases, and obtaining a target krypton component.

[0007] The one or more technical solutions provided in the present application have at least the following technical effects or advantages: The present application provides an air pre-purification control method and system for Kr enrichment separation. Through the synergistic operation of air pre-purification, multi-stage enrichment separation, and chromatographic separation, efficient enrichment and precise purification of krypton gas are realized. First, the air to be treated is pre-purified. By detecting the attribute characteristic information of the air, an operation parameter configurator of the purification device is constructed to obtain the adaptive purification operation parameters, and then the purification device is configured to remove the easily icing impurity components to obtain the purified air. Then, the purified air is subjected to multi-stage enrichment separation, and is sequentially passed through a first-stage and a second-stage enrichment separation unit. Each unit goes through the stages of adsorption, separation, and desorption. The temperature gradient control and carrier gas desorption combination are used to gradually increase the concentration of krypton gas, and the Kr-rich gas is obtained. Finally, the Kr-rich gas is input into a chromatographic separation device, and the adsorption-desorption difference of the chromatographic column stationary phase is used to separate krypton and other inert gases, and the target krypton component is obtained.

[0008] The technical solutions of the present application solve the problems of poor purification effect and unstable process caused by impurity icing blockage, low enrichment efficiency, and incomplete separation in traditional Kr enrichment separation by fusing multiple steps such as dynamic parameter configuration of air pre-purification, gradient purification of multi-stage enrichment separation, and precise separation of chromatographic separation. Efficient and stable Kr enrichment separation is realized, providing technical support for obtaining high-purity krypton gas. BRIEF DESCRIPTION OF DRAWINGS

[0009] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following will briefly introduce the drawings needed to be used in the embodiment description. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creating any inventive labor.

[0010] Figure 1 A flowchart of a Kr enrichment separation air pre-purification control method provided by the embodiments of the present application is shown. Figure 2 A structure diagram of a Kr enrichment separation air pre-purification control system provided by the embodiments of the present application is shown.

[0011] In the drawings, the components represented by the numbers are described as follows: Air pre-purification treatment module 01, multi-stage Kr enrichment separation module 02, chromatographic separation and purification module 03. DETAILED DESCRIPTION

[0012] The application provides an air pre-purification control method and system for Kr enrichment separation, which is used to solve the technical problems of fixed purification operation parameters, easy device blockage caused by difficulty in adapting to impurity changes, incomplete Kr adsorption and low separation purity caused by single multi-stage separation parameters in the prior art.

[0013] The technical solutions in the embodiments of the application will be clearly and completely described below with reference to the drawings in the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the application.

[0014] In the description of the application, the terms "first", "second" are used only for the purpose of description, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first", "second" can explicitly or implicitly include one or more of the features. In the description of the application, the meaning of "multiple" is two or more, unless otherwise specifically limited.

[0015] In the description of the application, the term "for example" is used to indicate "as an example, illustration or description". Any embodiment described as "for example" in the application is not necessarily interpreted as more preferred or more advantageous than other embodiments. The following description is given to enable any person skilled in the art to implement and use the application. In the following description, details are listed for the purpose of explanation. It should be understood that those skilled in the art can realize the application without using these specific details. In other examples, well-known structures and processes will not be described in detail to avoid unnecessary details making the description of the application obscure. Therefore, the application is not intended to be limited to the shown embodiments, but is consistent with the broadest scope of principles and characteristics disclosed in the application.

[0016] Embodiment one, as shown in the accompanying Figure 1 The application provides an air pre-purification control method for Kr enrichment separation, which comprises the following steps: S110: passing the air to be treated through a purification device to remove impurity components prone to icing in the air to be treated, and obtaining purified air; In the embodiments of the application, in the pre-treatment scenario of Kr enrichment separation, to avoid the blockage of the device by impurities prone to icing in subsequent low-temperature treatment, precise purification is achieved by dynamic parameter configuration.

[0017] Specifically, the attribute characteristic information of the to-be-processed air entering the impurity removal device is detected, and the detection includes key parameters such as temperature, humidity, and concentration of easily frozen impurities.

[0018] Further, for a specific model of the impurity removal device, historical high-quality impurity removal records of the same model device are collected, the attribute characteristics of the sample air and the corresponding optimal operation parameters are extracted, and the operation parameter configurator is trained based on this, so that the configurator can output adaptive impurity removal operation parameters according to the input real-time air attribute characteristics.

[0019] Finally, the impurity removal device is configured with the operation parameters, and efficient removal of the easily frozen impurities is completed, and clean impurity removal processed air is obtained.

[0020] This step provides a stable gas source basis for subsequent multi-stage enrichment separation through the technical solution of dynamic parameter optimization, and guarantees the continuous operation of the entire Kr enrichment separation process.

[0021] The step S110 in the method provided in the embodiment of the application includes: detecting attribute characteristic information of the to-be-processed air; constructing an operation parameter configurator of the impurity removal device, processing the attribute characteristic information through the operation parameter configurator, and obtaining impurity removal operation parameters; configuring the impurity removal device with the impurity removal operation parameters, removing the easily frozen impurity components in the to-be-processed air through the configured impurity removal device, and obtaining impurity removal processed air.

[0022] In the embodiment of the application, to achieve accurate removal of the easily frozen impurities, an operation parameter configurator needs to be constructed based on the impurity removal device, and dynamic impurity removal operation parameters are configured to adapt to changes in air attributes.

[0023] Specifically, the attribute characteristic information of the to-be-processed air entering the impurity removal device is detected, and the detection includes key parameters such as temperature, humidity, and concentration of easily frozen impurities (such as H2O and CO2).

[0024] For example, for a certain model of impurity removal device, the temperature of the to-be-processed air can be detected as 25°C, the humidity as 60%, and the CO2 concentration as 400 ppm.

[0025] Further, the operation parameter configurator is constructed based on the device model of the impurity removal device to analyze and process the attribute information of the to-be-processed air, so as to obtain adaptive impurity removal operation parameters.

[0026] The step of "constructing the operation parameter configurator of the impurity removal device" in the method provided in the embodiment of the application includes: obtaining the device model of the impurity removal device; Collect a plurality of historical high-quality impurity removal records of the same type of device based on the device model, including a plurality of attribute characteristic information of pre-treatment air of samples and a plurality of sample running parameters; Take the plurality of attribute characteristic information of pre-treatment air of samples as input features, and take the plurality of sample running parameters as supervision signals to train and obtain the running parameter configurator.

[0027] In the embodiments of the present application, when constructing the running parameter configurator, the model of the impurity removal device is taken as a reference to ensure accurate matching of the parameter configuration and the device characteristics.

[0028] Specifically, first, the model information of the current impurity removal device is read through the device identification, and the inherent attributes such as hardware specifications and processing capacity are determined to delimit the scope for subsequent data collection.

[0029] Further, based on the model, historical high-quality impurity removal records of the same type of device are collected from the device operation database. Each record contains attribute characteristic information (such as temperature, humidity, H2O and CO2 concentration, etc.) of pre-treatment air of samples and sample running parameters (such as impurity removal pressure, flow rate, adsorbent replacement period, etc.).

[0030] Among them, the historical high-quality impurity removal records are obtained by screening records of the same type of device in past operation, in which the residual amount of easily icing impurities in the air after impurity removal is less than 0.01%, and the device does not have blockage or efficiency reduction caused by icing of impurities.

[0031] For example, for an impurity removal device with a model of CZ-Kr500, 200 sets of historical high-quality records are selected from the database, one of which shows that the pre-treatment air temperature is 28°C, the humidity is 70%, the H2O concentration is 1.2 g / m³, and the CO2 concentration is 450 ppm.

[0032] At the same time, its corresponding running parameters are impurity removal pressure 0.35 MPa, flow rate 1.2 m / s, and adsorbent replacement period 8 hours. After processing by the parameters, the residual amount of easily icing impurities is only 0.008%, and the device has no blockage for 30 days of continuous operation, meeting the high-quality record standard.

[0033] Further, based on these historical high-quality impurity removal records, a random forest algorithm is selected as a basic framework to construct the running parameter configurator, and through the learning ability of integrating multiple decision trees, the mapping relationship between air attribute characteristics and impurity removal running parameters is analyzed.

[0034] Specifically, the attribute characteristic information (temperature, humidity, H2O concentration, CO2 concentration, etc.) of the air before sample processing is taken as the input feature, and the sample operation parameters (impurity removal pressure, flow rate, adsorbent replacement period, etc.) are taken as the supervision signal. The model is trained through a random sampling mechanism (random sampling of samples and random selection of features), so that the configurator can automatically adapt to the parameter optimization requirements under different air conditions.

[0035] First, 200 sets of sample data are divided into a training set (140 sets), a validation set (40 sets), and a test set (20 sets) in a 7:2:1 ratio, covering various working conditions such as high temperature and high humidity, low temperature and low humidity, to ensure the comprehensiveness of data distribution.

[0036] Further, in the model training stage, the initial number of decision trees is set to 30, and 80% of the samples in the training set are randomly selected each time. Three input single decision trees are randomly selected from four attribute characteristics. Taking impurity removal pressure prediction as an example, the decision tree learns the optimal value of the parameter under different feature combinations by recursive splitting (such as dividing the node with humidity > 60%).

[0037] Further, every time 10 decision trees are added, the model performance is evaluated using the validation set. For example, when the initial number of trees is 30, the validation set parameter prediction error is 0.05 MPa (pressure) and 0.1 m / s (flow rate). When the number of decision trees increases to 80, the error decreases to 0.02 MPa and 0.05 m / s.

[0038] At the same time, an early stopping mechanism is implemented. If the validation set error fluctuates by less than 0.005 for three consecutive rounds, the training is stopped. For example, when the number of decision trees reaches 80, the error stabilizes within 0.02 MPa for three consecutive rounds, and the model is determined to be converged.

[0039] Further, in the test stage, the test set is input into the model. If the average deviation of each parameter prediction value and the actual value is less than 0.03 MPa (pressure) and 0.08 m / s (flow rate), the operation parameter configurator is determined to be qualified and can be put into actual use.

[0040] Finally, the trained operation parameter configurator can output adaptive operation parameters according to real-time air attribute characteristics, provide dynamic control basis for the impurity removal device, and ensure the efficiency and stability of impurity removal.

[0041] Exemplarily, when the real-time attribute features of the air to be treated are temperature 32℃, humidity 68%, H2O concentration 1.1 g / m³, and CO2 concentration 430 ppm, these information is input into the trained operation parameter configurator, and the model outputs the impurity removal pressure 0.36 MPa, the flow rate 1.18 m / s, and the adsorbent replacement period 8 hours through the integrated calculation of multiple decision trees. It is verified through actual operation that the residual amount of the icing impurities under this parameter is 0.007%, the device is continuously operated for 30 days without blockage, the impurity removal effect is stable, and meets the expected requirements.

[0042] Further, after the training of the operation parameter configurator is completed, the impurity removal operation parameters output by the operation parameter configurator are applied to the actual regulation and control of the impurity removal device to realize the efficient removal of the icing impurities.

[0043] Specifically, the impurity removal pressure, flow rate, adsorbent replacement period and other parameters output by the operation parameter configurator are converted into executable instructions of the impurity removal device, and the core components such as valve opening, fan power, timer and the like are regulated and set through the control system of the device.

[0044] Exemplarily, if the impurity removal pressure output by the operation parameter configurator is 0.36 MPa, the control system will adjust the inlet valve opening to the corresponding threshold value to stabilize the internal pressure of the device at this value; and for the flow rate parameter of 1.18 m / s, the air flow speed is precisely controlled by adjusting the fan frequency.

[0045] Meanwhile, during the operation of the device, the outlet gas state of the impurity removal device is monitored in real time, including the icing impurity concentration, air flow stability and other indicators, to verify the effectiveness of the parameter configuration.

[0046] Finally, after the operation parameter configuration, the impurity removal device is continuously and stably operated to remove the icing impurities in the air to be treated to the target level, and outputs clean impurity removal treated air to provide qualified raw gas source for subsequent multi-stage enrichment separation of Kr.

[0047] S120: performing multi-stage enrichment separation treatment on the impurity removal treated air to obtain enriched Kr gas; In the embodiment of the present application, in the core stage of Kr enrichment separation, in order to realize efficient enrichment and precise purification of krypton, the enrichment efficiency needs to be improved through the differential temperature regulation of the multi-stage separation units.

[0048] Specifically, the impurity removal treated air is sequentially introduced into the first-stage and second-stage enrichment separation units, each unit is operated in three stages of adsorption, separation and desorption, and the krypton-containing gas desorbed from the previous stage is used as the input of the next stage. Finally, the enriched Kr gas with higher purity is output from the second-stage unit.

[0049] Firstly, in the adsorption stage, the input gas is adsorbed to adsorb the krypton therein at the corresponding adsorption temperature.

[0050] The adsorption temperature can be flexibly set according to the functional differences of the two-stage units. The first-stage unit focuses on mass adsorption, and a slightly higher first adsorption temperature can be used to achieve rapid adsorption; the second-stage unit focuses on fine enrichment, and a lower second adsorption temperature can be used to improve the adsorption efficiency.

[0051] Further, in the separation stage, the temperature is raised to the corresponding separation temperature, and other gas components adsorbed are separated and removed. That is, the first-stage unit is raised to the first separation temperature, and the second-stage unit is raised to the second separation temperature, and different types of impurities are removed by gradient heating.

[0052] Further, in the desorption stage, the temperature is raised to the corresponding desorption temperature, and the krypton is desorbed and output by the carrier gas. Similarly, the first-stage unit is raised to the first desorption temperature, and the second-stage unit is raised to the second desorption temperature, so that the krypton is separated from the adsorption material and enters the next stage of processing.

[0053] Finally, the first-stage unit takes the impurity-removed air as input, and the desorbed krypton-containing gas is output as input of the second-stage unit, and after fine processing by the second-stage unit, a Kr-enriched gas with higher purity is obtained.

[0054] This step realizes gradient enrichment of krypton gas by multi-stage differential parameter regulation and carrier gas desorption, and lays a foundation for subsequent chromatographic separation.

[0055] The step S120 in the method provided in the embodiments of the present application includes: The impurity-removed air is sequentially passed through the multi-stage enrichment separation units to obtain the Kr-enriched gas, wherein each enrichment separation unit includes an adsorption stage, a separation stage and a desorption stage; In the adsorption stage, the input gas is adsorbed to adsorb the krypton therein at the adsorption temperature. In the separation stage, the temperature is raised to the separation temperature, and other gas components adsorbed are separated and removed. In the desorption stage, the temperature is raised to the desorption temperature, and the krypton is desorbed and output by the carrier gas. The input of the first-stage enrichment separation unit is the impurity-removed air, the input of each subsequent enrichment separation unit is the krypton-containing gas output in the desorption stage of the previous stage, and the Kr-enriched gas is output in the desorption stage of the last stage.

[0056] In the embodiments of the present application, in order to realize efficient enrichment of krypton gas, the multi-stage separation units need to be operated cooperatively, and the temperature gradient and carrier gas desorption are combined to gradually improve the purity of krypton gas.

[0057] Specifically, the impurity-removed air is sequentially introduced into multiple enrichment separation units to obtain the enriched Kr gas. Each enrichment separation unit includes adsorption, separation and desorption stages.

[0058] Firstly, in the adsorption stage, the input gas passes through the adsorption device at the adsorption temperature, and the krypton is retained by the selective adsorption characteristics of the adsorption material, laying the foundation for subsequent separation and purification.

[0059] Then, in the separation stage, the adsorbed other gas components are desorbed and separated by being heated to the separation temperature, so that most of the interfering components are removed to increase the relative content of krypton.

[0060] Finally, in the desorption stage, the adsorbed krypton is desorbed and output by being heated to the desorption temperature with a carrier gas, so that the separation of krypton and the adsorption material is realized, and a gas with a higher krypton concentration is obtained and provided as input for the next unit.

[0061] In the embodiments of the present application, the adsorption temperature is -196°C, the separation temperature is -100°C, and the desorption temperature is 0°C. In the method provided by the embodiments of the present application, the step of "sequentially introducing the impurity-removed air into multiple enrichment separation units to obtain the enriched Kr gas" includes: introducing the impurity-removed air into a first enrichment separation unit for first enrichment separation to obtain a first enriched gas; introducing the first enriched gas into a second enrichment separation unit for second enrichment separation to obtain the enriched Kr gas.

[0062] In the embodiments of the present application, in order to realize gradient enrichment and purity improvement of krypton gas, a two-stage enrichment separation mode is adopted, and the krypton gas concentration is improved by optimizing the separation parameters step by step.

[0063] Specifically, the first enrichment separation unit takes the impurity-removed air as input, and after the adsorption, separation and desorption stages, the interfering components in the air are mainly removed, and a first enriched krypton-containing gas is obtained.

[0064] The step of "introducing the impurity-removed air into the first enrichment separation unit for first enrichment separation to obtain the first enriched gas" includes: adsorbing krypton in the impurity-removed air at a first adsorption temperature, separating and removing oxygen and nitrogen by being heated to a first separation temperature, and desorbing and obtaining the first enriched gas by being heated to a first desorption temperature; In the embodiments of the present application, the first enrichment separation unit is the initial link of multi-stage enrichment, and mainly realizes the preliminary capture of krypton and the removal of main impurities by temperature gradient regulation, thereby laying the foundation for subsequent second enrichment.

[0065] Specifically, first, the impurity-removed air is introduced into the adsorption device of the primary enrichment separation unit, and at a set first adsorption temperature, the krypton in the air is adsorbed and retained by the selective adsorption property of the adsorption material, and other gases are partially passed through or weakly adsorbed.

[0066] The first adsorption temperature can be set according to the processing efficiency requirement, and can be -196℃ to enhance the adsorption effect, or a slightly higher temperature (such as -180℃) to increase the processing speed.

[0067] Further, after the adsorption is completed, the separation stage is entered, and the adsorbed main gas components such as oxygen and nitrogen in the adsorption device are desorbed and separated by being raised to a first separation temperature, which can remove a large number of interference components and reduce the subsequent processing load.

[0068] The first separation temperature is usually set to a range that can effectively separate oxygen and nitrogen, for example, about -100℃.

[0069] Finally, the desorption stage is entered, and the temperature is continuously raised to a first desorption temperature, and a carrier gas (such as helium) is introduced to purge the adsorption device, so that the adsorbed krypton is desorbed and removed with the carrier gas, and a primary enrichment gas is obtained.

[0070] The first desorption temperature is generally set to 0℃, and at this temperature, krypton can be efficiently desorbed by combining with carrier gas purging.

[0071] For example, after the impurity-removed air enters the primary unit, the adsorption of krypton is completed at a first adsorption temperature of -196℃, then the temperature is raised to -100℃ to separate and remove oxygen and nitrogen, and then the temperature is raised to 0℃ and purged with 50ml of helium, and the krypton concentration in the primary enrichment gas obtained by desorption is significantly increased, and the oxygen and nitrogen content is greatly reduced, meeting the input requirements of the secondary enrichment separation.

[0072] In addition, the step of "carrying out secondary enrichment separation on the primary enrichment gas through a secondary enrichment separation unit to obtain the enriched Kr gas" includes: adsorbing the krypton in the primary enrichment gas at a second adsorption temperature, raising the temperature to a second separation temperature to separate and remove residual other gas components, and raising the temperature to a second desorption temperature to desorb and obtain the enriched Kr gas.

[0073] In the embodiments of the present application, the secondary enrichment separation unit is a deepening link of multi-stage enrichment, and through more precise temperature control, the krypton is deeply enriched and the residual impurities are accurately removed, and finally the enriched Kr gas with high purity is obtained.

[0074] Specifically, first, the primary enriched gas enters the adsorption stage, and is introduced into the adsorption device of the secondary enrichment separation unit. At a set second adsorption temperature, the krypton in the primary enriched gas is further adsorbed and retained by using the stronger selective adsorption capacity of the adsorption material for krypton, so as to reduce the interference of residual impurities.

[0075] The second adsorption temperature can be set according to the enrichment accuracy requirement. The second adsorption temperature can be consistent with the first adsorption temperature (for example, -196°C) to strengthen the adsorption effect, or a lower temperature (for example, -205°C) can be selected to improve the adsorption selectivity for krypton.

[0076] Further, after the adsorption is completed, the separation stage is entered, and the adsorbed residual other gas components (such as trace inert gas) in the adsorption device are desorbed and separated by being heated to a second separation temperature. This process can remove the residual interference components after the primary enrichment, so as to improve the purity of krypton.

[0077] The second separation temperature is usually set to an interval that can effectively separate the residual impurities, and can be adjusted according to the types of residual impurities. For example, the second separation temperature is slightly lower than or equal to the first separation temperature.

[0078] Finally, the desorption stage is entered, the temperature is continuously increased to a second desorption temperature, and a carrier gas (such as helium) is introduced to purge the adsorption device, so that the adsorbed high-purity krypton is desorbed and detached and is output with the carrier gas to obtain the enriched Kr gas.

[0079] Similarly, the second desorption temperature is also set to 0°C, and at this temperature, the carrier gas is purged to ensure efficient desorption and collection of krypton.

[0080] For example, after the primary enriched gas enters the secondary unit, the deep adsorption of krypton is completed at a second adsorption temperature of -196°C, then the temperature is increased to -100°C to separate and remove residual other gas components, and then the temperature is increased to 0°C and the obtained enriched Kr gas is purged with 50 ml of helium. The krypton concentration in the enriched Kr gas obtained by desorption is greatly improved, the content of residual impurities is lower, and the input requirements of subsequent chromatographic separation are met.

[0081] S130: introducing the enriched Kr gas into a chromatographic separation device to separate krypton and other inert gases and obtain a target krypton component.

[0082] In the embodiment of the present application, after the multi-stage enrichment of krypton gas is completed, the high-efficiency separation capability of the chromatographic separation device is used to further realize the accurate separation of krypton and other inert gases, and finally a high-purity target krypton component is obtained.

[0083] Specifically, the enriched Kr gas obtained through multi-stage enrichment is introduced into a chromatographic separation device (such as a TCD chromatograph), which uses 5A molecular sieve as a chromatographic column stationary phase, utilizes the adsorption-desorption capacity difference of different inert gases in the stationary phase, and realizes the separation of the mixed gas in the chromatographic column by the carrier gas.

[0084] Among them, because of the difference in molecular structure and polarity between krypton and other inert gases (such as xenon, argon, etc.), the retention time of krypton in the chromatographic column is different, so it can be eluted out in turn.

[0085] Further, the gas components eluted out are monitored and analyzed in real time by a chromatographic detector, and the krypton component is accurately identified and collected according to the peak time and peak area of the characteristic peak.

[0086] For example, when the enriched Kr gas enters the chromatographic separation device, under certain chromatographic conditions (such as column temperature, carrier gas flow rate, etc.), krypton will form a characteristic peak in a preset time window. By controlling the fraction collection device, the effluent in this time period can be collected to obtain high-purity target krypton component.

[0087] This step is the final link of the Kr enrichment and separation process. Through the high selectivity and high resolution of chromatographic separation technology, the complete separation of krypton and other inert gases is realized, ensuring that the target krypton component can meet the purity requirements of subsequent applications.

[0088] Through the above specific embodiments, the following technical effects are achieved: The application provides an air pre-purification control method for Kr enrichment and separation. First, the air to be treated is pre-purified. By detecting its temperature, humidity, and easy-to-freeze impurity concentration, etc. attribute characteristic information, the operation parameter configurator of the purification device is constructed to obtain the adaptive purification operation parameters, and then the purification device is configured to remove the easy-to-freeze impurity components to obtain the purified air, which provides a clean gas source for subsequent enrichment and separation. Then, the purified air is subjected to multi-stage enrichment and separation, and is sequentially passed through a first-stage and a second-stage enrichment and separation unit. Each unit operates in three stages of adsorption, separation, and analysis. The temperature gradient control combined with carrier gas analysis is used to gradually increase the krypton gas concentration to obtain enriched Kr gas. Finally, the enriched Kr gas is introduced into a chromatographic separation device to separate krypton from other inert gases by the adsorption-desorption difference of the 5A molecular sieve chromatographic column, and high-purity target krypton component is obtained by detection and collection.

[0089] The method provided by the embodiment of the application solves the problems of poor purification effect and unstable process caused by device blockage due to impurity icing, low enrichment efficiency and incomplete separation in traditional Kr enrichment and separation, realizes efficient enrichment and accurate purification of krypton, and provides reliable technical support for obtaining high-purity krypton.

[0090] Embodiment two, as shown in the attached Figure 2 Based on the inventive concept of the air pre-impurity removal control method for Kr enrichment and separation provided in embodiment one, the application further provides an air pre-impurity removal control system for Kr enrichment and separation, which specifically comprises: An air pre-impurity removal treatment module 01 is configured to pass the air to be treated through an impurity removal device to remove the impurity components prone to icing in the air to be treated, thereby obtaining impurity-removed air; A multi-stage Kr enrichment and separation module 02 is configured to perform multi-stage enrichment and separation treatment on the impurity-removed air, thereby obtaining enriched Kr gas; A chromatographic separation and purification module 03 is configured to pass the enriched Kr gas into a chromatographic separation device to separate krypton and other inert gases, thereby obtaining target krypton components.

[0091] In one embodiment, the air pre-impurity removal treatment module 01 is further configured to: detect attribute characteristic information of the air to be treated; construct an operation parameter configurator of the impurity removal device, process the attribute characteristic information through the operation parameter configurator, and obtain impurity removal operation parameters; configure the impurity removal device with the impurity removal operation parameters, remove the impurity components prone to icing in the air to be treated through the configured impurity removal device, and obtain impurity-removed air.

[0092] In one embodiment, the multi-stage Kr enrichment and separation module 02 is further configured to: pass the impurity-removed air through multi-stage enrichment and separation units in sequence to obtain the enriched Kr gas, wherein each enrichment and separation unit includes an adsorption stage, a separation stage and a desorption stage; in the adsorption stage, input gas is adsorbed by an adsorption device at an adsorption temperature to adsorb krypton therein; in the separation stage, the temperature is raised to a separation temperature to separate and remove other gas components that are adsorbed; in the desorption stage, the temperature is raised to a desorption temperature, and krypton is desorbed and output by a carrier gas; wherein the input of the first-stage enrichment and separation unit is the impurity-removed air, the input of each subsequent enrichment and separation unit is the krypton-containing gas output from the desorption stage of the previous stage, and the enriched Kr gas is output from the desorption stage of the last stage.

[0093] It should be noted that the above-mentioned embodiment sequences of the present application are merely for description, and do not represent the advantages and disadvantages of the embodiments. And the above describes the specific embodiments of the present application. In addition, the processes depicted in the drawings do not necessarily require the specific order or continuous order shown to achieve the desired results. In some embodiments, multi-task processing and parallel processing are also possible or can be advantageous.

[0094] The above only describes the preferred embodiments of the present application, and does not limit the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

[0095] The specification and drawings are merely exemplary of the present application, and any and all modifications, variations, combinations or equivalents that fall within the scope of the present application should be included. Obviously, those skilled in the art can make various modifications and variations to the present application without departing from the scope of the present application. Thus, if these modifications and variations of the present application belong to the scope of the present application and its equivalents, the present application is intended to include these modifications and variations.

Claims

1. A method for controlling air pre-removal for Kr enrichment and separation, characterized in that, The method includes: The air to be treated is passed through a purification device to remove impurities that are prone to freezing, thus obtaining purified air. The air that has undergone impurity removal treatment is subjected to multi-stage enrichment and separation treatment to obtain enriched Kr gas; The enriched Kr gas is passed into a chromatographic separation device to separate krypton and other inert gases, thereby obtaining the target krypton component.

2. The method according to claim 1, characterized in that, The air to be treated is passed through a purification device to remove easily icing impurities, resulting in purified air, including: Detect the property characteristics of the air to be processed; A configuration tool for the operating parameters of the impurity removal device is constructed, and the attribute feature information is processed through the configuration tool to obtain the impurity removal operating parameters; The impurity removal device is configured with the aforementioned impurity removal operating parameters. By removing easily icing impurity components from the air to be treated, impurity-removed air is obtained.

3. The method according to claim 2, characterized in that, Constructing the operating parameter configurator for the impurity removal device includes: Obtain the device model of the impurity removal device; Based on the device model, multiple historical high-quality impurity removal records of the same model device were collected, including the property characteristics of the air before multiple sample processing and multiple sample operating parameters; Using the air property characteristics information of the multiple samples before processing as input features and the operating parameters of the multiple samples as supervision signals, the operating parameter configurator is trained and obtained.

4. The method according to claim 1, characterized in that, The air undergoes multi-stage enrichment and separation processing to obtain enriched Kr gas, including: The air that has undergone impurity removal is passed through a multi-stage enrichment and separation unit in sequence to obtain the enriched Kr gas. Each enrichment and separation unit includes an adsorption stage, a separation stage, and a desorption stage. During the adsorption stage, the input gas is passed through an adsorption device at the adsorption temperature to adsorb krypton. In the separation stage, the temperature is raised to the separation temperature to separate and remove other adsorbed gaseous components; During the desorption stage, the temperature is raised to the desorption temperature, and the krypton is desorbed and desorbed using a carrier gas. The first-stage enrichment and separation unit receives the purified air as input, the subsequent enrichment and separation units receive the krypton-containing gas output from the previous analysis stage, and the final analysis stage outputs the enriched Kr gas.

5. The method according to claim 4, characterized in that, The adsorption temperature is -196℃, the separation temperature is -100℃, and the desorption temperature is 0℃.

6. The method according to claim 4, characterized in that, The purified air is sequentially passed through a multi-stage enrichment and separation unit to obtain the enriched Kr gas, including: The air that has undergone impurity removal is subjected to primary enrichment and separation in a primary enrichment and separation unit to obtain primary enriched gas. The primary enriched gas is subjected to secondary enrichment and separation by a secondary enrichment and separation unit to obtain the enriched Kr gas.

7. The method according to claim 6, characterized in that, The air undergoing impurity removal is passed through a primary enrichment and separation unit to obtain a primary enriched gas, comprising: Krypton is adsorbed from the air in the purification treatment at the first adsorption temperature, oxygen and nitrogen are separated and removed by heating to the first separation temperature, and the primary enriched gas is obtained by desorption and desorption at the first desorption temperature. The primary enriched gas is further enriched and separated by a secondary enrichment and separation unit to obtain the enriched Kr gas, comprising: Krypton in the primary enriched gas is adsorbed at the second adsorption temperature, and the remaining gas components are removed by heating to the second separation temperature. The enriched Kr gas is obtained by desorption by heating to the second desorption temperature.

8. An air pre-removal control system for Kr enrichment and separation, characterized in that, The system is used to execute the air pre-removal control method for Kr enrichment and separation according to any one of claims 1-7, the system comprising: An air pre-removal module is used to pass the air to be treated through a removal device to remove impurities that are prone to freezing, thereby obtaining air with impurities removed. A multi-stage Kr enrichment and separation module is used to perform multi-stage enrichment and separation processing on the air that has undergone impurity removal to obtain Kr-enriched gas. The chromatographic separation and purification module is used to pass the enriched Kr gas into a chromatographic separation device to separate krypton and other inert gases to obtain the target krypton component.

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