CN-116952482-B - Inner U-shaped adsorption column inner leakage detection system and method

CN116952482BCN 116952482 BCN116952482 BCN 116952482BCN-116952482-B

Abstract

The invention relates to an adsorption column tightness test system and a test method, in particular to an inner U-shaped adsorption column inner leakage detection system and an inner leakage detection method, which are used for solving the defect that a detection method suitable for inner U-shaped adsorption column inner leakage detection does not exist at present. The internal U-shaped adsorption column internal leakage detection system comprises a gas configuration device, a constant temperature device, a detection analysis device and a pressure monitoring device, wherein the system can select different analysis and measurement methods according to different target components, can accurately and quantitatively analyze in a laboratory, can also be used for carrying out portable detection in factories, workshops or outdoors, has limited influence of impurity components on target component detection results, and can also be used for correcting temperature influence, so that the system has wide environmental adaptability and practicability. Meanwhile, the invention discloses an inner leakage detection method of the inner U-shaped adsorption column.

Inventors

ZHOU CHONGYANG
ZHOU GUOQING
WU RUI
GONG BING
FENG SHUJUAN

Assignees

西北核技术研究所

Dates

Publication Date: 20260505
Application Date: 20220420

Claims (7)

1. The internal U-shaped adsorption column internal leakage detection system is characterized by comprising a gas configuration device, a constant temperature device (2), a detection analysis device (3) and a pressure monitoring device; The gas configuration device comprises a first gas device (11) and a second gas device (12) which are connected in parallel, wherein the first gas device (11) comprises a first gas source (111), a first pressure reducing valve (112), a first mass flow controller (113) and a first valve (114) which are sequentially arranged along the gas flow direction and connected through a pipeline, the second gas device (12) comprises a second gas source (121), and a second pressure reducing valve (122), a second mass flow controller (123) and a second valve (124) which are sequentially arranged along the gas flow direction and connected through a pipeline, the first gas in the first gas source (111) does not contain a target component of an adsorbent, the second gas in the second gas source (121) contains a target component of the adsorbent, mixed gas is formed after the first gas and the second gas are configured, and the target component content in the mixed gas is higher than the detection limit of the detection analysis device (3); The constant temperature device (2) is used for keeping a constant temperature of the U-shaped adsorption column (01) in the to-be-detected, an adsorbent is filled in the U-shaped adsorption column (01) in the to-be-detected, two ends of the U-shaped adsorption column (01) in the to-be-detected are respectively provided with a gas inlet (011) and a gas outlet (012), a first outlet of the gas configuration device is connected with a first exhaust pipeline (52), a third valve (521) is arranged at an outlet of the first exhaust pipeline (52), a second outlet of the gas configuration device is connected with a first pipeline (51), an outlet of the first pipeline (51) is connected with the gas inlet (011), and a fourth valve (511) is arranged on the first pipeline (51); The gas outlet (012) is connected with an inlet of a second pipeline (53), a fifth valve (531) and a third mass flowmeter (532) for detecting the flow rate of mixed gas are sequentially arranged on the second pipeline (53) along the gas flow direction, a first outlet of the second pipeline (53) is connected with a second exhaust pipeline (54), a seventh valve (541) is arranged at an outlet of the second exhaust pipeline (54), a third pipeline (56) is connected at a second outlet of the second pipeline (53), an outlet of the third pipeline (56) is connected with an inlet of the detection and analysis device (3), a sixth valve (561) is arranged on the third pipeline (56) close to the detection and analysis device (3), and a third exhaust pipeline (55) is connected with an outlet of the detection and analysis device (3), and the detection and analysis device (3) is used for measuring the content of a target component and determining whether a column body of the U-shaped adsorption column (01) in a to be detected is qualified or not according to the ventilation time and the flow rate of the third mass flowmeter (532); The pressure monitoring device comprises a first pressure sensor (41) located in the first pipeline (51) and close to the gas inlet (011), a second pressure sensor (42) located in the second pipeline (53) and close to the gas outlet (012), and a third pressure sensor (43) located in the third pipeline (56) and close to the inlet of the detection analysis device (3).
2. The internal U-shaped adsorption column internal leakage detection system according to claim 1, wherein the adsorbent is one or more mixtures, and the target component is one or more mixtures.
3. An inner U-shaped adsorption column inner leakage detection method is characterized in that an inner U-shaped adsorption column inner leakage detection system as claimed in claim 1 is adopted, and comprises the following steps: Step1, drying an adsorbent; Drying the adsorbent, and cooling for later use; step 2, measuring the volume of the U-shaped adsorption column (01) in the sample; Cleaning the inside of the U-shaped adsorption column (01) to be detected for multiple times, then injecting liquid to test the volume of the U-shaped adsorption column (01) to be detected, and drying the U-shaped adsorption column (01) to be detected for later use; Step 3, (3.1) Weighing the U-shaped adsorption column (01) to be detected treated in the step (2), filling the adsorbent treated in the step (1), and weighing again to obtain the adsorbent loading W; (3.2) according to the formula 1, combining the adsorbent loading W and a constant value k (T, P) corresponding to a target component of the adsorbent at a preset temperature T and a preset pressure P to obtain a relation between a preset penetration time T 5％ of the target component to the detection analysis device (3) and a preset mixed gas flow Q, and estimating the preset mixed gas flow Q according to a value range of T 5％ ; the preset temperature T is the constant temperature of the constant temperature device (2), and the preset pressure P is the average value of the pressure of the first pressure sensor (41) and the pressure of the second pressure sensor (42); (3.3) according to formula 2, combining the preset mixed gas flow rate Q, the standard gas concentration C 0 of the second gas source (121) and the mixed gas concentration C f to obtain a preset flow rate Q 2 of the second mass flow controller (123); (3.4) calculating a preset flow rate Q 1 of the first mass flow controller (113) according to formula 3 in combination with the preset mixed gas flow rate Q and the flow rate Q 2 of the second mass flow controller (123); q 1 ＝Q-Q 2 equation 3 Step 4, checking the leakage of the inner U-shaped adsorption column (01) to be checked; (4.1) if the U-shaped adsorption column (01) in the test is known to have no leakage, executing the step 5, otherwise, executing the step (4.2); (4.2) opening a first pressure reducing valve (112), setting the flow of a first mass flow controller (113) to be a preset flow Q 1 , opening a first valve (114) and a fourth valve (511), closing the first valve (114) and the fourth valve (511) after the pressures of a first pressure sensor (41) and a second pressure sensor (42) reach 300kPa, waiting for more than 1 hour, recording the pressure of the first pressure sensor (41), if the value change of the first pressure sensor (41) is less than 1kPa, indicating that the U-shaped adsorption column (01) in the test is not leaked, executing step 5, otherwise, indicating that the U-shaped adsorption column (01) in the test is leaked, and ending the flow; step 5, cleaning the adsorbent; Opening a constant temperature device (2) and setting constant temperature, opening a first valve (114), a fourth valve (511) and a fifth valve (531), unscrewing a seventh valve (541) to the maximum, keeping the flow of a first mass flow controller (113) unchanged at a preset flow Q 1 , and ventilating and cleaning the column body of the U-shaped adsorption column (01) to be detected for more than 12 hours; Step 6, background detection; Opening a detection analysis device (3), opening a sixth valve (561), and reducing a seventh valve (541), so that the pressure of a third pressure sensor (43) is increased by more than a preset pressure difference than that of the step 5, and the outflow gas of a U-shaped adsorption column (01) in the to-be-detected enters the detection analysis device (3) and is maintained for more than 0.5 hour; When the detection analysis device (3) detects that the content of the target component in the gas flowing out of the U-shaped adsorption column (01) in the to-be-detected is lower than the detection limit, executing the step 7; step 7, target component adsorption; The opening degree of the first valve (114), the opening degree of the sixth valve (561) and the opening degree of the seventh valve (541) are kept unchanged, the opening degree of the fourth valve (511) and the opening degree of the fifth valve (531) are closed, the second valve (124) and the third valve (521) are opened, the flow rate of the first mass flow controller (113) is kept unchanged at a preset flow rate Q 1 , the flow rate of the second mass flow controller (123) is regulated, after the flow rate is stable, the fourth valve (511) and the fifth valve (531) are opened and the ventilation time is recorded, mixed gas enters the U-shaped adsorption column (01) to be detected, the adsorbent adsorbs target components, and the outflow gas of the U-shaped adsorption column (01) to be detected enters the detection analysis device (3); step 8, measuring the penetration time t x(5％) ; The detection and analysis device (3) continuously analyzes the gas flowing out of the U-shaped adsorption column (01) in the to-be-detected at the same time interval, when a target component signal S x appears, the analysis is continued until the value of S x is not changed any more, the final value of S x is recorded as S f , and the ending time is recorded; Step 9, data processing; Processing the target component signals S x and S f in the step 8, respectively converting into concentrations C x and C f by using a standard curve formula of the detection and analysis device (3), drawing a penetration curve with time on the abscissa and C x /C f on the ordinate, obtaining the corresponding actual penetration time t x(5％) when C x /C f =5%, comparing with the preset penetration time t 5％ , if t x(5％) ＜t 5％ , indicating that the U-shaped adsorption column (01) in the detection has internal leakage, otherwise, indicating that the internal leakage condition of the U-shaped adsorption column (01) in the detection accords with the use standard.
4. The method for detecting the internal leakage of the U-shaped adsorption column according to claim 3, further comprising the step of 10, judging the internal leakage of the U-shaped adsorption column with the same size; Processing the target component signals S x and S f in the step 8, respectively converting into the concentrations C x and C f by using a standard curve formula of a detection analysis device, drawing a penetration curve with the abscissa being time and the ordinate being C x /C f , and obtaining the actual penetration time corresponding to each inner U-shaped adsorption column when C x /C f = 5% N is the corresponding ordinal number of each inner U-shaped adsorption column; If a certain occurs Significantly smaller than the rest Description of the embodiment The corresponding inner U-shaped adsorption column is provided with an inner leakage.
5. The method for detecting leakage in an inner U-shaped adsorption column according to claim 3, wherein in the step (3.2), the value range of t 5％ is 30-60 min.
6. The method for detecting leakage in an inner U-shaped adsorption column according to claim 4 or 5, wherein in step 6, the preset pressure difference is 0.2kPa.
7. The method for detecting leakage in an inner U-shaped adsorption column according to claim 6, wherein in step 8, the time interval is 5min.

Description

Inner U-shaped adsorption column inner leakage detection system and method Technical Field The invention relates to an adsorption column tightness test system and a test method, in particular to an inner U-shaped adsorption column inner leakage detection system and an inner leakage detection method. Background The adsorption column is a core component of the gas adsorption separation device, and the size of the adsorption column directly determines the performance index, operation, structure and layout of the adsorption column. The adsorption column generally adopts an inner 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 the inner U-shaped adsorption column has inner leakage, the system experimental result is obviously affected, so that the inner leakage detection of the adsorption column with high efficiency and operability is very necessary. In the prior art, there are many methods for detecting leakage, such as helium mass spectrometry, soap foam or pressure, but the methods cannot be used for detecting leakage in an inner U-shaped adsorption column. Disclosure of Invention The invention aims to solve the defect that a detection method suitable for detecting the inner leakage of an inner U-shaped adsorption column does not exist at present, and provides an inner U-shaped adsorption column inner leakage detection system and method. In order to solve the defects existing in the prior art, the invention provides the following technical solutions: the inner leakage detection system of the inner U-shaped adsorption column is characterized by comprising a gas configuration device, a constant temperature device, a detection analysis device and a pressure monitoring device; The gas configuration device comprises a first gas device and a second gas device which are connected in parallel, wherein the first gas device comprises a first gas source, a first pressure reducing valve, a first mass flow controller and a first valve which are sequentially arranged along the gas flow direction and connected through a pipeline, the second gas device comprises a second gas source, a second pressure reducing valve, a second mass flow controller and a second valve which are sequentially arranged along the gas flow direction and connected through a pipeline, the first gas in the first gas source does not contain a target component of an adsorbent, the second gas in the second gas source contains a target component of the adsorbent, mixed gas is formed after the first gas and the second gas are configured, and the content of the target component in the mixed gas is higher than the detection limit of the detection analysis device; The constant temperature device is used for keeping the constant temperature of the U-shaped adsorption column to be detected, an adsorbent is filled in the U-shaped adsorption column to be detected, and the two ends of the U-shaped adsorption column to be detected are respectively provided with a gas inlet and a gas outlet; the gas outlet is connected with an inlet of a second pipeline, a fifth valve and a third mass flowmeter for detecting the flow of mixed gas are sequentially arranged on the second pipeline along the gas flowing direction, a first outlet of the second pipeline is connected with a second exhaust pipeline, a seventh valve is arranged at an outlet of the second exhaust pipeline, a second outlet of the second pipeline is connected with a third pipeline, an outlet of the third pipeline is connected with an inlet of the detection and analysis device, a sixth valve is arranged on the third pipeline close to the inlet of the detection and analysis device, and an outlet of the detection and analysis device is connected with the third exhaust pipeline; The pressure monitoring device comprises a first pressure sensor, a second pressure sensor and a third pressure sensor, wherein the first pressure sensor is positioned on the first pipeline and is close to the gas inlet, the second pressure sensor is positioned on the second pipeline and is close to the gas outlet, and the third pressure sensor is positioned on the third pipeline and is close to the inlet of the detection analysis device. Further, the adsorbent is one or more of mixture, and the target component is one or more of mixture. Meanwhile, the invention also provides an inner leakage detection method of the inner U-shaped adsorption column, which is characterized by comprising the following steps of: Step1, drying an adsorbent; Drying the adsorbent, and cooling for later use; step 2, measuring the volume of the U-shaped adsorption column to be detected; cleaning the inside of the U-shaped adsorption column to be detected for multiple times, then injecting liquid to test the volume of the U-shaped adsorption column to be detected, and then drying the U-shaped adsorption column to be detected for later use; Step 3,