A system and method for detecting leaks in an inner U-shaped adsorption column

By combining a gas preparation device, a constant temperature device, and a pressure monitoring device, and utilizing the selective adsorption characteristics of the adsorbent, rapid and non-destructive detection of internal leakage in the inner U-shaped adsorption column is achieved, solving the problem of internal leakage detection in the inner U-shaped adsorption column and making it suitable for various environments.

CN116952482BActive Publication Date: 2026-05-05NORTHWEST INST OF NUCLEAR TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
NORTHWEST INST OF NUCLEAR TECH
Filing Date
2022-04-20
Publication Date
2026-05-05

AI Technical Summary

Technical Problem

The lack of an effective method for detecting internal leakage in existing U-shaped adsorption columns makes internal leakage detection difficult.

Method used

Using a gas preparation device, a temperature control device, a detection and analysis device, and a pressure monitoring device, internal leakage is determined by the selective adsorption of the mixed gas and the breakthrough time. Combined with pressure monitoring, internal leakage detection of the inner U-shaped adsorption column is achieved.

Benefits of technology

This invention provides a simple, low-cost, and portable method for detecting internal leakage in U-shaped adsorption columns, suitable for use in laboratories, factories, and the field. It can quickly determine the degree of internal leakage without damaging the adsorption column.

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Patent Text Reader

Abstract

The present application relates to a kind of inner U type adsorption column leakage detection system and leakage detection method, and it is used to solve the deficiency of the detection method for inner U type adsorption column leakage detection at present.The inner U type adsorption column leakage detection system includes gas configuration device, thermostat device, detection analysis device and pressure monitoring device, the system can select different analysis measurement methods according to different target components, both can be accurately quantitative analysis in laboratory, also can be portable detection in factory, workshop or field, impurity component has limited influence on target component detection result, temperature influence can also be corrected, therefore, it has wide environmental adaptability and practicality.At the same time, the present application discloses a kind of inner U type adsorption column leakage detection method.
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Description

Technical Field

[0001] This invention relates to an adsorption column sealing test system and test method, specifically to an internal leakage detection system and method for an internal U-shaped adsorption column. Background Technology

[0002] The adsorption column is the core component of a gas adsorption separation device, and its size directly determines its performance indicators, operation, structure, and layout. Adsorption columns typically employ an internal U-shaped structure, which not only reduces the size and weight of the gas adsorption separation device but also maintains high adsorption column efficiency. However, if an internal leak exists in the internal U-shaped adsorption column, it will significantly affect the experimental results of the system. Therefore, effective and operable internal leak detection of adsorption columns is essential. In existing technologies, there are many methods for detecting external leaks, such as helium mass spectrometry, soap frothing, or pressure, but none of these methods can be used for detecting internal leaks in internal U-shaped adsorption columns. Summary of the Invention

[0003] The purpose of this invention is to address the current lack of a suitable detection method for detecting internal leakage in an internal U-shaped adsorption column, and to provide an internal leakage detection system and method for an internal U-shaped adsorption column.

[0004] To address the shortcomings of the existing technology, the present invention provides the following technical solution:

[0005] A leak detection system for an internal U-shaped adsorption column is characterized by including a gas preparation device, a temperature control device, a detection and analysis device, and a pressure monitoring device.

[0006] The gas preparation device includes a first gas device and a second gas device connected in parallel. The first gas device includes a first gas source, and a first pressure reducing valve, a first mass flow controller, and a first valve arranged sequentially along the gas flow direction and connected by a pipeline. The second gas device includes a second gas source, and a second pressure reducing valve, a second mass flow controller, and a second valve arranged sequentially along the gas flow direction and connected by a pipeline. The first gas in the first gas source does not contain the target component of the adsorbent, and the second gas in the second gas source contains the target component of the adsorbent. The first gas and the second gas are prepared to form a mixed gas, and the content of the target component in the mixed gas is higher than the detection limit of the detection and analysis device.

[0007] The constant temperature device is used to maintain a constant temperature in the U-shaped adsorption column to be tested. The U-shaped adsorption column to be tested is filled with adsorbent, and the two ends of the U-shaped adsorption column to be tested are a gas inlet and a gas outlet, respectively. The first outlet of the gas preparation device is connected to a first exhaust pipe, and the outlet of the first exhaust pipe is equipped with a third valve. The second outlet of the gas preparation device is connected to a first pipe, the outlet of the first pipe is connected to the gas inlet, and a fourth valve is installed on the first pipe.

[0008] The gas outlet is connected to the inlet of the second pipeline. A fifth valve and a third mass flow meter for detecting the flow rate of the mixed gas are sequentially installed on the second pipeline along the gas flow direction. The first outlet of the second pipeline is connected to a second exhaust pipeline. A seventh valve is installed at the outlet of the second exhaust pipeline. The second outlet of the second pipeline is connected to a third pipeline. The outlet of the third pipeline is connected to the inlet of the detection and analysis device. A sixth valve is installed on the third pipeline near the inlet of the detection and analysis device. The outlet of the detection and analysis device is connected to the third exhaust pipeline. The detection and analysis device is used to determine the content of the target component and, in conjunction with the ventilation time and the flow rate of the third mass flow meter, to determine whether the U-shaped adsorption column to be tested is qualified.

[0009] The pressure monitoring device includes a first pressure sensor located in the first pipeline and near the gas inlet, a second pressure sensor located in the second pipeline and near the gas outlet, and a third pressure sensor located in the third pipeline and near the inlet of the detection and analysis device.

[0010] Furthermore, the adsorbent is one or more types or a mixture thereof; the target component is one or more types or a mixture thereof.

[0011] Meanwhile, the present invention also provides a method for detecting internal leakage in an inner U-shaped adsorption column, which is characterized by employing the above-mentioned internal U-shaped adsorption column internal leakage detection system and includes the following steps:

[0012] Step 1: Drying the adsorbent;

[0013] After drying the adsorbent, cool it for later use.

[0014] Step 2: Measure the volume of the U-shaped adsorption column to be tested;

[0015] The inside of the U-shaped adsorption column to be tested was cleaned multiple times, then liquid was injected to test the volume of the U-shaped adsorption column to be tested, and then the U-shaped adsorption column to be tested was dried for later use.

[0016] Step 3

[0017] (3.1) Weigh the U-shaped adsorption column to be tested after step 2, fill it with the adsorbent after step 1, weigh it again, and obtain the adsorbent loading W.

[0018] (3.2) According to Formula 1, combined with the adsorbent loading W and the constant value k(T,P) corresponding to the target component of the adsorbent at the preset temperature T and preset pressure P, the preset breakthrough time t for the target component to reach the detection and analysis device is obtained. 5% The relationship between the flow rate and the preset mixed gas flow rate Q is based on t. 5% The range of values ​​is used to estimate the preset mixed gas flow rate Q;

[0019]

[0020] The preset temperature T is the constant temperature of the thermostat, and the preset pressure P is the average of the pressure from the first pressure sensor and the pressure from the second pressure sensor.

[0021] (3.3) According to Formula 2, combined with the preset mixed gas flow rate Q, the standard gas concentration of the second gas source C0, and the mixed gas concentration C f The preset flow rate Q2 of the second mass flow controller is obtained;

[0022]

[0023] (3.4) According to Formula 3, the preset flow rate Q1 of the first mass flow controller is calculated by combining the preset mixed gas flow rate Q and the flow rate Q2 of the second mass flow controller;

[0024] Q1=Q-Q2 Formula 3

[0025] Step 4: Check for external leakage of the U-shaped adsorption column to be inspected;

[0026] (4.1) If it is known that there is no external leakage in the U-shaped adsorption column to be tested, then proceed to step 5; otherwise, proceed to step (4.2).

[0027] (4.2) Open the first pressure reducing valve, set the flow rate of the first mass flow controller to the preset flow rate Q1, and open the first valve and the fourth valve; when the pressure of the first pressure sensor and the second pressure sensor both reach 300 kPa, close the first valve and the fourth valve; wait for more than 1 hour, record the pressure of the first pressure sensor, if the change in the value of the first pressure sensor is less than 1 kPa, it means that there is no external leakage in the U-shaped adsorption column to be tested, and proceed to step 5; otherwise, it means that there is external leakage in the U-shaped adsorption column to be tested, and end the process;

[0028] Step 5: Cleaning the adsorbent;

[0029] Turn on the thermostat and set a constant temperature. Open the first valve, the fourth valve and the fifth valve. Turn the seventh valve to the maximum. Keep the flow rate of the first mass flow controller at the preset flow rate Q1. Clean the U-shaped adsorption column to be inspected by ventilation for more than 12 hours.

[0030] Step 6: Background detection;

[0031] Turn on the detection and analysis device, open the sixth valve, and turn the seventh valve to make the pressure of the third pressure sensor higher than the preset pressure difference in step 5, so as to ensure that the gas flowing out of the U-shaped adsorption column to be tested enters the detection and analysis device and remains there for more than 0.5 hours.

[0032] When the detection and analysis device detects that the content of the target component in the gas flowing out of the U-shaped adsorption column is lower than the detection limit, proceed to step 7;

[0033] Step 7: Adsorption of the target component;

[0034] Keep the openings of the first, sixth, and seventh valves unchanged, close the fourth and fifth valves, open the second and third valves, keep the flow rate of the first mass flow controller at the preset flow rate Q1, adjust the flow rate of the second mass flow controller, and after the flow rate stabilizes, open the fourth and fifth valves and record the ventilation time; the mixed gas enters the U-shaped adsorption column to be tested, the adsorbent adsorbs the target component, and the gas flowing out of the U-shaped adsorption column to be tested enters the detection and analysis device;

[0035] Step 8, Penetration time t x(5%) Measurement;

[0036] The detection and analysis device continuously analyzes the gas effluent from the U-shaped adsorption column under test at the same time intervals. When the target component signal S appears... x Continue the analysis until S x S will be moved until the value no longer changes. x The final value is denoted as S. f Record the end time; close all valves, temperature control devices and detection and analysis devices to complete the monitoring of the breakthrough time of the target component in the U-shaped adsorption column to be tested;

[0037] Step 9: Data processing;

[0038] For the target component signal S in step 8 x and S f The samples were processed and converted to concentration C using the standard curve formula of the detection and analysis device. x and C f Plot a graph with time on the x-axis and C on the y-axis. x / C f The penetration curve yields C. x / C f The actual penetration time t corresponding to 5% x(5%) , and the preset penetration time t 5% In comparison; if t x(5%) <t 5% If the test result is positive, it indicates that the U-shaped adsorption column under test has internal leakage; otherwise, it indicates that the internal leakage condition of the U-shaped adsorption column under test meets the usage standards.

[0039] Furthermore, it also includes step 10, determining leakage within U-shaped adsorption columns of the same size;

[0040] For multiple inner U-shaped adsorption columns with the same size as the inner U-shaped adsorption column to be tested in step 9, perform steps 4 to 8; for the target component signal S in step 8x and S f The samples were processed and converted to concentration C using the standard curve formula of the detection and analysis device. x and C f Plot a graph with time on the x-axis and C on the y-axis. x / C f The penetration curve yields C. x / C f Actual breakthrough time of each inner U-shaped adsorption column at 5% n is the ordinal number of each inner U-shaped adsorption column;

[0041] If a certain Significantly smaller than the rest Explain this The corresponding internal U-shaped adsorption column has internal leakage.

[0042] Further, in step (3.2), the t 5% The value range is 30 min to 60 min.

[0043] Furthermore, in step 6, the preset pressure difference is 0.2 kPa.

[0044] Furthermore, in step 8, the time interval is 5 minutes.

[0045] Compared with the prior art, the beneficial effects of the present invention are:

[0046] (1) The present invention provides an internal leakage detection system for an internal U-shaped adsorption column, comprising a gas preparation device, a constant temperature device, a detection and analysis device, and a pressure monitoring device. The principle of the system is based on the selective adsorption of the target component by the adsorbent, and the determination of whether the path has changed according to the time it takes to reach the measuring device, thereby determining whether there is an internal leakage. The system can select different analysis and measurement methods according to different target components, and can accurately quantify in the laboratory, or conduct portable detection in factories, workshops, or in the field. The influence of impurity components on the detection results of the target components is limited, and the influence of temperature can also be corrected. Therefore, it has wide environmental adaptability and practicality.

[0047] (2) The present invention provides a method for detecting internal leakage in an inner U-shaped adsorption column, which can select one or more candidate target components or a variety of different adsorbents to meet the needs of different inner U-shaped adsorption columns. This method does not damage the inner U-shaped adsorption column and has the advantages of simple operation and low cost.

[0048] (3) The present invention provides a method for detecting internal leakage of an inner U-shaped adsorption column, which can be used for detecting internal leakage of multiple inner U-shaped adsorption columns of the same size. The method can quickly determine the degree of internal leakage by comparing the penetration time. Attached Figure Description

[0049] Figure 1 This is a schematic diagram of an embodiment of an internal leakage detection system for an internal U-shaped adsorption column according to the present invention.

[0050] The markings on the attached diagram of the U-shaped adsorption column to be tested are explained below:

[0051] 01-U-shaped adsorption column to be tested, 011-Gas inlet, 012-Gas outlet;

[0052] 11-First gas device, 111-First gas source, 112-First pressure reducing valve, 113-First mass flow controller, 114-First valve, 12-Second gas device, 121-Second gas source, 122-Second pressure reducing valve, 123-Second mass flow controller, 124-Second valve;

[0053] 2-Thermostatic device;

[0054] 3-Detection and analysis device;

[0055] 41-First pressure sensor, 42-Second pressure sensor, 43-Third pressure sensor;

[0056] 51-First pipeline, 511-Fourth valve, 52-First exhaust pipeline, 521-Third valve, 53-Second pipeline, 531-Fifth valve, 532-Third mass flow meter, 54-Second exhaust pipeline, 541-Seventh valve, 55-Third exhaust pipeline, 56-Third pipeline, 561-Sixth valve. Detailed Implementation

[0057] The present invention will be further described below with reference to the accompanying drawings and exemplary embodiments.

[0058] Reference Figure 1 A leak detection system for an internal U-shaped adsorption column includes a gas preparation device, a constant temperature device 2, a detection and analysis device 3, and a pressure monitoring device.

[0059] The gas preparation device includes a first gas device 11 and a second gas device 12 connected in parallel. The first gas device 11 includes a first gas source 111, and a first pressure reducing valve 112, a first mass flow controller 113, and a first valve 114 arranged sequentially along the gas flow direction and connected by pipelines. The second gas device 12 includes a second gas source 121, and a second pressure reducing valve 122, a second mass flow controller 123, and a second valve 124 arranged sequentially along the gas flow direction and connected by pipelines. In this embodiment, the first gas in the first gas source 111 is nitrogen, which does not contain the target component of the adsorbent. The second gas in the second gas source 121 contains the target component of the adsorbent. The first gas and the second gas are prepared to form a mixed gas. The content of the target component in the mixed gas is higher than the detection limit of the detection and analysis device 3.

[0060] The constant temperature device 2 is used to keep the U-shaped adsorption column 01 under test at a constant temperature. The U-shaped adsorption column 01 under test is filled with adsorbent. The two ends of the U-shaped adsorption column 01 under test are a gas inlet 011 and a gas outlet 012, respectively.

[0061] The first outlet of the gas preparation device is connected to a first exhaust pipe 52, and a third valve 521 is installed at the outlet of the first exhaust pipe 52; the second outlet of the gas preparation device is connected to a first pipe 51, and the outlet of the first pipe 51 is connected to a gas inlet 011, and a fourth valve 511 is installed on the first pipe 51.

[0062] Gas outlet 012 is connected to the inlet of the second pipeline 53. A fifth valve 531 and a third mass flow meter 532 for detecting the flow rate of the mixed gas are sequentially installed on the second pipeline 53 along the gas flow direction. The first outlet of the second pipeline 53 is connected to a second exhaust pipeline 54. A seventh valve 541 is installed at the outlet of the second exhaust pipeline 54. The second outlet of the second pipeline 53 is connected to a third pipeline 56. The outlet of the third pipeline 56 is connected to the inlet of the detection and analysis device 3. A sixth valve 561 is installed on the third pipeline 56 near the detection and analysis device 3. The outlet of the detection and analysis device 3 is connected to a third exhaust pipeline 55. The detection and analysis device 3 is used to determine the content of the target component and, in conjunction with the ventilation time and the flow rate of the third mass flow meter 532, to determine whether the column of the U-shaped adsorption column 01 to be tested is qualified.

[0063] The pressure monitoring device includes a first pressure sensor 41 located in the first pipeline 51 and near the gas inlet 011, a second pressure sensor 42 located in the second pipeline 53 and near the gas outlet 012, and a third pressure sensor 43 located in the third pipeline 56 and near the inlet of the detection and analysis device 3.

[0064] Based on the above-mentioned internal leakage detection system of internal U-shaped adsorption column, the present invention provides an internal leakage detection method of internal U-shaped adsorption column. The principle is based on the selective adsorption of target component by adsorbent, and judging whether its path changes according to the time it takes to reach the measuring device, thereby judging whether there is internal leakage.

[0065] The method for detecting internal leakage in an internal U-shaped adsorption column includes the following steps:

[0066] Step 1: Drying the adsorbent;

[0067] The adsorbent was placed in an oven at 100°C and dried for at least 24 hours. After being removed, it was placed in a desiccator to cool and store for later use.

[0068] Step 2: Measure the volume of the U-shaped adsorption column 01 to be tested;

[0069] The inside of the U-shaped adsorption column 01 to be tested was cleaned with distilled water several times. Then, liquid was injected to test the volume of the U-shaped adsorption column 01 to be tested. Finally, the U-shaped adsorption column 01 to be tested was dried for later use.

[0070] Step 3

[0071] (3.1) Weigh the U-shaped adsorption column 01 to be tested after step 2, fill it with the adsorbent after step 1, weigh it again, and obtain the adsorbent loading W.

[0072] (3.2) According to Formula 1, combined with the adsorbent loading W and the constant value k(T,P) corresponding to the target component of the adsorbent at the preset temperature T and preset pressure P, the preset breakthrough time t for the target component to reach the detection and analysis device 3 is obtained. 5% The relationship between t and the preset mixed gas flow rate Q 5% The value ranges from 30 min to 60 min, and the preset mixed gas flow rate Q is estimated accordingly.

[0073]

[0074] The preset temperature T is the constant temperature of the constant temperature device 2, and the preset pressure P is the average of the pressure of the first pressure sensor 41 and the pressure of the second pressure sensor 42.

[0075] (3.3) According to Formula 2, combined with the preset mixed gas flow rate Q and the standard gas concentration C0 (ppm) of the second gas source 121, the mixed gas concentration C is assumed to be... f The value is 50ppm, and the preset flow rate Q2 of the second mass flow controller 123 is obtained;

[0076]

[0077] (3.4) According to Formula 3, the preset flow rate Q1 of the first mass flow controller 113 is calculated by combining the preset mixed gas flow rate Q and the flow rate Q2 of the second mass flow controller 123;

[0078] Q1=Q-Q2 Formula 3

[0079] Step 4: Check for external leakage of the U-shaped adsorption column 01 to be inspected;

[0080] (4.1) If it is known that there is no external leakage in the U-shaped adsorption column (01) to be tested, then proceed to step 5; otherwise, proceed to step (4.2).

[0081] (4.2) Open the first pressure reducing valve 112, set the flow rate of the first mass flow controller 113 to the preset flow rate Q1, and open the first valve 114 and the fourth valve 511; when the pressure of the first pressure sensor 41 and the second pressure sensor 42 both reach 300 kPa, close the first valve 114 and the fourth valve 511; wait for 1 hour and record the pressure of the first pressure sensor 41. If the change in the value of the first pressure sensor 41 is less than 1 kPa, it indicates that there is no external leakage in the U-shaped adsorption column 01 to be tested, and proceed to step 5; otherwise, it indicates that there is external leakage in the U-shaped adsorption column 01 to be tested, and end the process.

[0082] Step 5: Cleaning the adsorbent;

[0083] Turn on the thermostat 2 and set the constant temperature to 25°C. Open the first valve 114, the fourth valve 511 and the fifth valve 531. Turn the seventh valve 541 to the maximum. Keep the flow rate of the first mass flow controller 113 at the preset flow rate Q1. Clean the U-shaped adsorption column 01 to be inspected by ventilation for 12 hours.

[0084] Step 6: Background detection;

[0085] Turn on the detection and analysis device 3, open the sixth valve 561, and turn the seventh valve 541 to make the pressure of the third pressure sensor 43 increase by 0.2 kPa compared with step 5, so as to ensure that the gas flowing out of the U-shaped adsorption column 01 to be tested enters the detection and analysis device 3 and is maintained for 0.5 hours.

[0086] When the detection and analysis device 3 detects that the content of the target component in the gas flowing out of the U-shaped adsorption column 01 is lower than the detection limit, step 7 is executed.

[0087] Step 7: Adsorption of the target component;

[0088] Keep the openings of the first valve 114, the sixth valve 561, and the seventh valve 541 unchanged, close the fourth valve 511 and the fifth valve 531, open the second valve 124 and the third valve 521, keep the flow rate of the first mass flow controller 113 at the preset flow rate Q1 unchanged, adjust the flow rate of the second mass flow controller 123, and after the flow rate stabilizes, open the fourth valve 511 and the fifth valve 531 and record the ventilation time; the mixed gas enters the U-shaped adsorption column 01 to be tested, the adsorbent adsorbs the target component, and the gas flowing out of the U-shaped adsorption column 01 to be tested enters the detection and analysis device 3;

[0089] Step 8, Penetration time t x(5%) Measurement;

[0090] The detection and analysis device 3 continuously analyzes the gas flowing out of the U-shaped adsorption column 01 at the same time intervals. When the target component signal S appears... x Continue the analysis until S x S will be moved until the value no longer changes. x The final value is denoted as S. f Record the end time; close all valves, thermostat 2 and detection and analysis device 3, and the breakthrough time monitoring of the target component in the U-shaped adsorption column 01 to be tested is completed;

[0091] Step 9: Data processing;

[0092] For the target component signal S in step 8 x and S f The samples were processed and converted to concentration C using the standard curve formula of the detection and analysis device 3. x and C f Plot a graph with time on the x-axis and C on the y-axis. x / C f The penetration curve yields C. x / C f Actual penetration time corresponding to 5% t x (5%) , and the preset penetration time t 5% In comparison; if t x(5%) <t 5% If the test result is positive, it indicates that the U-shaped adsorption column 01 under test has internal leakage; otherwise, it indicates that the internal leakage condition of the U-shaped adsorption column 01 under test meets the usage standards.

[0093] Step 10: Leakage detection of U-shaped adsorption columns of the same size;

[0094] For multiple inner U-shaped adsorption columns with the same size as the inner U-shaped adsorption column 01 to be tested in step 9, perform steps 4 to 8; for the target component signal S in step 8 x and S fThe samples were processed and converted to concentration C using the standard curve formula of the detection and analysis device. x and C f Plot a graph with time on the x-axis and C on the y-axis. x / C f The penetration curve yields C. x / C f Actual breakthrough time of each inner U-shaped adsorption column at 5% n is the ordinal number of each inner U-shaped adsorption column;

[0095] If a certain Significantly smaller than the rest Explain this The corresponding internal U-shaped adsorption column has internal leakage.

[0096] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit them. For those skilled in the art, modifications can be made to the specific technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. However, these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions protected by the present invention.

Claims

1. A leak detection system for an internal U-shaped adsorption column, characterized in that: It includes a gas preparation device, a constant temperature device (2), a detection and analysis device (3), and a pressure monitoring device; The gas configuration device includes a first gas device (11) and a second gas device (12) connected in parallel. The first gas device (11) includes a first gas source (111), and a first pressure reducing valve (112), a first mass flow controller (113), and a first valve (114) arranged sequentially along the gas flow direction and connected by a pipeline. The second gas device (12) includes a second gas source (121), and a second pressure reducing valve (122), a second mass flow controller (123), and a second valve (124) arranged sequentially along the gas flow direction and connected by a pipeline. The first gas in the first gas source (111) does not contain the target component of the adsorbent, and the second gas in the second gas source (121) contains the target component of the adsorbent. The first gas and the second gas are configured to form a mixed gas, and the content of the target component in the mixed gas is higher than the detection limit of the detection and analysis device (3). The constant temperature device (2) is used to keep the U-shaped adsorption column (01) under test at a constant temperature. The U-shaped adsorption column (01) under test is filled with adsorbent. The two ends of the U-shaped adsorption column (01) under test are a gas inlet (011) and a gas outlet (012), respectively. The first outlet of the gas preparation device is connected to a first exhaust pipe (52). The outlet of the first exhaust pipe (52) is equipped with a third valve (521). The second outlet of the gas preparation device is connected to a first pipe (51). The outlet of the first pipe (51) is connected to the gas inlet (011). The first pipe (51) is equipped with a fourth valve (511). The gas outlet (012) is connected to the inlet of the second pipeline (53). The second pipeline (53) is provided with a fifth valve (531) and a third mass flow meter (532) for detecting the flow rate of the mixed gas in sequence along the gas flow direction. The first outlet of the second pipeline (53) is connected to the second exhaust pipeline (54). The outlet of the second exhaust pipeline (54) is provided with a seventh valve (541). The second outlet of the second pipeline (53) is connected to the third pipeline (56). The outlet of the third pipeline (56) is connected to the inlet of the detection and analysis device (3). The third pipeline (56) is provided with a sixth valve (561) near the detection and analysis device (3). The outlet of the detection and analysis device (3) is connected to the third exhaust pipeline (55). The detection and analysis device (3) is used to determine the content of the target component and, in combination with the ventilation time and the flow rate of the third mass flow meter (532), determine whether the column of the U-shaped adsorption column (01) to be tested is qualified. The pressure monitoring device includes a first pressure sensor (41) located in the first pipeline (51) and near the gas inlet (011), a second pressure sensor (42) located in the second pipeline (53) and near the gas outlet (012), and a third pressure sensor (43) located in the third pipeline (56) and near the inlet of the detection and analysis device (3).

2. The internal leakage detection system of the U-shaped adsorption column according to claim 1, characterized in that: The adsorbent is one or more in combination; the target component is one or more in combination.

3. A method for detecting internal leakage in an internal U-shaped adsorption column, characterized in that, The internal leakage detection system of the U-shaped adsorption column according to claim 1 includes the following steps: Step 1: Drying the adsorbent; After drying the adsorbent, cool it for later use. Step 2: Volume measurement of the U-shaped adsorption column (01) to be tested; The inside of the U-shaped adsorption column (01) to be tested was cleaned multiple times. Then, liquid was injected to test the volume of the U-shaped adsorption column (01) to be tested. The U-shaped adsorption column (01) to be tested was then dried for later use. Step 3 (3.1) Weigh the U-shaped adsorption column (01) to be tested after step 2, fill it with the adsorbent after step 1, weigh it again, and obtain the adsorbent loading W. (3.2) According to Formula 1, combined with the adsorbent loading W and the constant value k(T,P) corresponding to the target component of the adsorbent at the preset temperature T and preset pressure P, the preset breakthrough time t of the target component to reach the detection and analysis device (3) is obtained. 5% The relationship between the flow rate and the preset mixed gas flow rate Q is based on t. 5% The range of values ​​is used to estimate the preset mixed gas flow rate Q; The preset temperature T is the constant temperature of the constant temperature device (2), and the preset pressure P is the average of the pressure of the first pressure sensor (41) and the pressure of the second pressure sensor (42). (3.3) According to Formula 2, combined with the preset mixed gas flow rate Q, the standard gas concentration C0 of the second gas source (121), and the mixed gas concentration C f The preset flow rate Q2 of the second mass flow controller (123) is obtained; (3.4) According to Formula 3, the preset flow rate Q1 of the first mass flow controller (113) is calculated by combining the preset mixed gas flow rate Q and the flow rate Q2 of the second mass flow controller (123); Q1=Q-Q2 Formula 3 Step 4: Check for external leakage of the U-shaped adsorption column (01) to be inspected; (4.1) If it is known that there is no external leakage in the U-shaped adsorption column (01) to be tested, then proceed to step 5; otherwise, proceed to step (4.2). (4.2) Open the first pressure reducing valve (112), set the flow rate of the first mass flow controller (113) to the preset flow rate Q1, and open the first valve (114) and the fourth valve (511); when the pressure of the first pressure sensor (41) and the second pressure sensor (42) both reach 300 kPa, close the first valve (114) and the fourth valve (511); wait for more than 1 hour, record the pressure of the first pressure sensor (41), if the change in the value of the first pressure sensor (41) is less than 1 kPa, it indicates that there is no external leakage in the U-shaped adsorption column (01) to be tested, and proceed to step 5; otherwise, it indicates that there is external leakage in the U-shaped adsorption column (01) to be tested, and end the process; Step 5: Cleaning the adsorbent; Turn on the thermostat (2) and set a constant temperature. Open the first valve (114), the fourth valve (511) and the fifth valve (531). Turn the seventh valve (541) to the maximum. Keep the flow rate of the first mass flow controller (113) at the preset flow rate Q1. Ventilate and clean the U-shaped adsorption column (01) to be inspected for more than 12 hours. Step 6: Background detection; Open the detection and analysis device (3), open the sixth valve (561), and reduce the seventh valve (541) to make the pressure of the third pressure sensor (43) increase by more than the preset pressure difference compared to step 5, so as to ensure that the gas flowing out of the U-shaped adsorption column (01) to be tested enters the detection and analysis device (3) and is maintained for more than 0.5 hours. When the detection and analysis device (3) detects that the content of the target component in the gas flowing out of the U-shaped adsorption column (01) is lower than the detection limit, step 7 is executed; Step 7: Adsorption of the target component; Keep the openings of the first valve (114), the sixth valve (561) and the seventh valve (541) unchanged, close the fourth valve (511) and the fifth valve (531), open the second valve (124) and the third valve (521), keep the flow rate of the first mass flow controller (113) at the preset flow rate Q1 unchanged, adjust the flow rate of the second mass flow controller (123), and after the flow rate stabilizes, open the fourth valve (511) and the fifth valve (531) and record the ventilation time; the mixed gas enters the U-shaped adsorption column (01) to be tested, the adsorbent adsorbs the target component, and the gas flowing out of the U-shaped adsorption column (01) to be tested enters the detection and analysis device (3); Step 8, Penetration time t x(5%) Measurement; The detection and analysis device (3) continuously analyzes the gas flowing out of the U-shaped adsorption column (01) at the same time intervals. When the target component signal S appears... x Continue the analysis until S x S will be moved until the value no longer changes. x The final value is denoted as S. f Record the end time; close all valves, the constant temperature device (2) and the detection and analysis device (3) to complete the monitoring of the breakthrough time of the target component in the U-shaped adsorption column (01) to be tested; Step 9: Data processing; For the target component signal S in step 8 x and S f The samples were processed and converted to concentration C using the standard curve formula of the detection and analysis device (3). x and C f Plot a graph with time on the x-axis and C on the y-axis. x / C f The penetration curve yields C. x / C f The actual penetration time t corresponding to 5% x(5%) , and the preset penetration time t 5% In comparison; if t x(5%) <t 5% If the test result is positive, it indicates that the U-shaped adsorption column (01) under test has internal leakage; otherwise, it indicates that the internal leakage condition of the U-shaped adsorption column (01) under test meets the usage standard.

4. The method for detecting internal leakage in an internal U-shaped adsorption column according to claim 3, characterized in that, It also includes: Step 10, leakage judgment of U-shaped adsorption columns of the same size; For multiple inner U-shaped adsorption columns with the same size as the inner U-shaped adsorption column (01) to be tested in step 9, perform steps 4 to 8; for the target component signal S in step 8 x and S f The samples were processed and converted to concentration C using the standard curve formula of the detection and analysis device. x and C f Plot a graph with time on the x-axis and C on the y-axis. x / C f The penetration curve yields C. x / C f Actual breakthrough time of each inner U-shaped adsorption column at 5% n is the ordinal number of each inner U-shaped adsorption column; If a certain Significantly smaller than the rest Explain this The corresponding internal U-shaped adsorption column has internal leakage.

5. The method for detecting internal leakage in an internal U-shaped adsorption column according to claim 3, characterized in that: In step (3.2), the t 5% The value range is 30 min to 60 min.

6. A method for detecting internal leakage in an inner U-shaped adsorption column according to claim 4 or 5, characterized in that: In step 6, the preset pressure difference is 0.2 kPa.

7. The method for detecting internal leakage in an internal U-shaped adsorption column according to claim 6, characterized in that: In step 8, the time interval is 5 minutes.

Citation Information

Patent Citations

  • Internal leakage detection device for adsorption tower

    CN217901126U