CN113188974A - High-pressure hydrogen permeation test device and method for liner material of IV-type gas cylinder - Google Patents
High-pressure hydrogen permeation test device and method for liner material of IV-type gas cylinder Download PDFInfo
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- CN113188974A CN113188974A CN202110482314.XA CN202110482314A CN113188974A CN 113188974 A CN113188974 A CN 113188974A CN 202110482314 A CN202110482314 A CN 202110482314A CN 113188974 A CN113188974 A CN 113188974A
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 118
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 118
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 238000012360 testing method Methods 0.000 title claims abstract description 81
- 239000007789 gas Substances 0.000 title claims abstract description 71
- 239000000463 material Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title abstract description 12
- 230000035699 permeability Effects 0.000 claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 112
- 229910052757 nitrogen Inorganic materials 0.000 claims description 55
- 238000010926 purge Methods 0.000 claims description 40
- 238000001816 cooling Methods 0.000 claims description 36
- 238000002955 isolation Methods 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 28
- 238000007789 sealing Methods 0.000 claims description 20
- 238000012544 monitoring process Methods 0.000 claims description 19
- 238000005485 electric heating Methods 0.000 claims description 14
- 239000011148 porous material Substances 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 230000008595 infiltration Effects 0.000 claims description 4
- 238000001764 infiltration Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000011144 upstream manufacturing Methods 0.000 claims description 2
- 238000010998 test method Methods 0.000 abstract description 11
- 238000009530 blood pressure measurement Methods 0.000 abstract description 3
- 238000009529 body temperature measurement Methods 0.000 abstract description 3
- 230000010354 integration Effects 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 description 5
- 229920001903 high density polyethylene Polymers 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
- G01N15/0826—Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
The invention provides a high-pressure hydrogen permeation test device and a high-pressure hydrogen permeation test method for liner materials of IV-type gas cylinders, wherein the high-pressure hydrogen permeation test device comprises the following steps: the airtight anchor clamps that combine with the sample, the air supply system that is linked together and the detecting system that is linked together with the sample opposite side with sample one side, wherein: the gas supply system comprises a gas supply pipeline communicated with the hydrogen cylinder group, the gas supply pipeline is connected to a gas inlet pipeline through a booster pump, and the gas inlet pipeline is closely communicated with one side surface of the sample; the detection system comprises an air outlet pipeline which is closely connected and communicated with the other side surface of the sample, and the air outlet pipeline is connected to a mass spectrometer I. The testing device and the testing method provided by the invention can systematically and accurately test the hydrogen permeability of different types of liner materials. Compared with the traditional test method, the method has the advantages that the test under constant test pressure can be realized, the test under circulating pressure can also be realized, the pressure measurement and temperature measurement range is wider, the functions are complete, the equipment integration level is high, and the like.
Description
Technical Field
The invention relates to a high-pressure hydrogen permeation test device and method for a composite gas cylinder plastic liner material, and belongs to the technical field of hydrogen energy storage and transportation equipment.
Background
The IV-type gas cylinder has become a main hydrogen storage device on a hydrogen fuel cell vehicle at present due to the advantages of high volume-weight ratio and high hydrogen storage density. The inner layer of the IV-type gas cylinder is usually made of HDPE, PA6 and other plastic materials through thermoforming to form a closed inner container, and the IV-type gas cylinder has the advantages of light weight, easiness in forming and corrosion resistance, has lower density than steel and aluminum in a microstructure, can enable hydrogen molecules to leak through the wall surface of the inner container when operated for a long time in a high-pressure hydrogen environment, forms hydrogen aggregation in an external closed space, and can possibly cause explosion risks after reaching a certain magnitude.
For the IV-type gas cylinder, the control of the hydrogen permeability by selecting a high-quality liner material is one of key technologies for safe use of the gas cylinder. The hydrogen permeability difference of different liner materials is large, so that the hydrogen permeability of the liner materials is measured when the materials are selected. The hydrogen permeation environment mainly experienced by the liner material is a circulating pressure permeation process of hydrogen charging and hydrogen utilization under an operating condition and a constant pressure permeation process under a non-operating condition, so that the material meeting the standard requirement is selected as the liner of the gas cylinder according to actual conditions.
At present, the research on the performance of the plastic liner material of the IV-type gas cylinder in the high-pressure hydrogen environment is still in an exploration stage in China, and particularly, a penetration test method under the circulating pressure is not yet mature. Through research and improvement of a test method, the hydrogen permeability of different types of liner materials is measured, so that test data of the different types of liner materials can be accumulated, a mature liner permeability evaluation method and a qualified index are formed, and a proper material is preferably selected as the liner of the IV-type gas cylinder, so that the method has extremely important significance.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art, provides a device and a method for testing the high-pressure hydrogen permeability of an IV-type gas cylinder liner material, and is beneficial to researching the performance of the IV-type gas cylinder plastic liner material in a high-pressure hydrogen environment.
In order to achieve the purpose, the invention adopts the technical scheme that:
the utility model provides a high pressure hydrogen permeation test device of IV type gas cylinder inner bag material which characterized in that includes: the airtight anchor clamps that combine with the sample, the air supply system that is linked together and the detecting system that is linked together with the sample opposite side with sample one side, wherein:
the gas supply system comprises a gas supply pipeline communicated with the hydrogen cylinder group, the gas supply pipeline is connected to a gas inlet pipeline through a booster pump, and the gas inlet pipeline is closely communicated with one side surface of the sample;
the detection system comprises an air outlet pipeline which is closely connected and communicated with the other side surface of the sample, and the air outlet pipeline is connected to a mass spectrometer I.
The IV-type gas cylinder liner material high-pressure hydrogen permeation test device comprises: and the periphery of the clamp is provided with a shielding cover which hermetically surrounds the clamp, the upper opening of the shielding cover is communicated with a bypass pipeline, and the bypass pipeline is connected to a second mass spectrometer.
The IV-type gas cylinder liner material high-pressure hydrogen permeation test device comprises: the gas supply pipeline is communicated with the hydrogen cylinder group and the nitrogen cylinder group in a switching mode, the bypass pipeline is communicated to a purging nitrogen source through a purging one-way valve, and the purging nitrogen source can send purging nitrogen into the isolation hood through the purging one-way valve.
The IV-type gas cylinder liner material high-pressure hydrogen permeation test device comprises: and an air release valve is arranged on the air inlet pipeline.
The IV-type gas cylinder liner material high-pressure hydrogen permeation test device comprises: and a buffer tank and an air supply control valve are sequentially arranged at the downstream of the booster pump of the air supply pipeline, and the air supply control valve is positioned at the upstream position of the emptying valve.
The IV-type gas cylinder liner material high-pressure hydrogen permeation test device comprises: the upper part and the lower part of the clamp are respectively fixed with an electric heating rod which is connected to a heating power supply; and cooling channels are arranged in the upper part and/or the lower part of the clamp and communicated to the cooling working medium circulation pipeline.
The IV-type gas cylinder liner material high-pressure hydrogen permeation test device comprises: and thermocouples are fixed on the upper part and/or the lower part of the clamp.
The IV-type gas cylinder liner material high-pressure hydrogen permeation test device comprises: and the system is also provided with a signal numerical control device which is in signal connection with the mass spectrometer I, the mass spectrometer II, the booster pump, the air supply control valve, the blow-down valve, the electric heating rod, the thermocouple, the cooling working medium circulating pipeline and the purging nitrogen source and is connected with the data processing device.
A hydrogen permeability test method under constant pressure uses the high-pressure hydrogen permeability test device for the liner material of the IV-type gas cylinder, and is characterized by comprising the following steps:
(1) sample preparation: placing a sample into a groove at the lower part of a clamp, placing a sintered metal mesh and an O-shaped sealing ring into the groove in advance, placing the O-shaped sealing ring at the upper part of the clamp, relatively fixing the upper part and the lower part of the clamp, and hermetically connecting the upper surface and the lower surface of the sample with the O-shaped sealing ring respectively;
(2) heating and cooling function selection:
when a high-temperature environment test is carried out, an electric heating rod is inserted into the side edge of the clamp, the cooling working medium circulation pipeline is disconnected, the isolation cover is covered, and a bypass pipeline on the isolation cover is connected to a second mass spectrometer; a heating power supply is switched on, and after the fixture is heated to the test temperature through the heating rod, the fixture is kept warm for a certain period of time;
when a low-temperature environment test is carried out, the heating rod is taken out, the heating rod is communicated with a cooling working medium circulation pipeline, the isolation cover is covered and communicated with a second mass spectrometer, and after the clamp is cooled to the test temperature through the cooling working medium circulation pipeline, the clamp is kept warm for a certain period of time;
(3) nitrogen replacement of the isolation cover and the air inlet pipeline: after the test temperature reaches the standard, connecting a purging nitrogen source, opening a vent valve, allowing nitrogen from the purging nitrogen source to enter the isolation hood through a purging one-way valve, and performing nitrogen purging replacement on the air inlet pipeline and the interior of the isolation hood respectively; meanwhile, the gas supply pipeline is switched to be communicated with the nitrogen cylinder group, so that the gas supply pipeline is replaced by nitrogen;
(4) constant pressurization and pressure maintaining: closing the air release valve, switching the air supply pipeline to be communicated with the hydrogen cylinder group, introducing hydrogen of the hydrogen cylinder group into the booster pump, and contacting the generated high-pressure hydrogen with the upper surface of the sample through the air inlet pipeline and the pore passage at the upper part of the clamp after the generated high-pressure hydrogen reaches the test pressure;
(5) and (3) detecting the hydrogen concentration: after maintaining the pressure for a period of time, starting hydrogen concentration detection: opening a mass spectrograph and No. two mass spectrometers simultaneously and carrying out the hydrogen monitoring, a mass spectrograph is used for monitoring the hydrogen of sample thickness direction infiltration, and No. two mass spectrometers are used for monitoring the hydrogen concentration of the sealed face leakage of anchor clamps.
A hydrogen permeability test method under circulating pressure uses the high-pressure hydrogen permeability test device for the liner material of the IV-type gas cylinder, and is characterized by comprising the following steps:
(1) sample preparation: placing a sample into a groove at the lower part of a clamp, placing a sintered metal mesh and an O-shaped sealing ring into the groove in advance, placing the O-shaped sealing ring at the upper part of the clamp, relatively fixing the upper part and the lower part of the clamp, and hermetically connecting the upper surface and the lower surface of the sample with the O-shaped sealing ring respectively;
(2) heating and cooling function selection:
when a high-temperature environment test is carried out, an electric heating rod is inserted into the side edge of the clamp, the cooling working medium circulation pipeline is disconnected, the isolation cover is covered, and a bypass pipeline on the isolation cover is connected to a second mass spectrometer; a heating power supply is switched on, and after the fixture is heated to the test temperature through the heating rod, the fixture is kept warm for a certain period of time;
when a low-temperature environment test is carried out, the heating rod is taken out, the heating rod is communicated with a cooling working medium circulation pipeline, the isolation cover is covered and communicated with a second mass spectrometer, and after the clamp is cooled to the test temperature through the cooling working medium circulation pipeline, the clamp is kept warm for a certain period of time;
(3) nitrogen replacement of the isolation cover and the air inlet pipeline: after the test temperature reaches the standard, connecting a purging nitrogen source, opening a vent valve, allowing nitrogen from the purging nitrogen source to enter the isolation hood through a purging one-way valve, and performing nitrogen purging replacement on the air inlet pipeline and the interior of the isolation hood respectively; meanwhile, the gas supply pipeline is switched to be communicated with the nitrogen cylinder group, so that the gas supply pipeline is replaced by nitrogen;
(4) pressure circulation: closing an air release valve, switching an air supply pipeline to be communicated with a hydrogen cylinder group, pressurizing hydrogen of the hydrogen cylinder group by a booster pump, then feeding the pressurized hydrogen into a buffer tank, enabling high-pressure hydrogen to be in contact with the upper surface of the sample through an air inlet pipeline and a hole channel at the upper part of the clamp, maintaining the pressure for several seconds, closing an air supply control valve, slowly opening the air release valve to release the pressure until the pressure is lower than a preset value, closing the air release valve, continuing for several seconds, and ending a pressure cycle; then opening the air supply control valve and continuously performing the next pressure cycle;
(5) hydrogen monitoring: a mass spectrometer and No. two mass spectrometers are opened simultaneously, and a mass spectrometer is used for monitoring the hydrogen of sample thickness direction infiltration, and No. two mass spectrometers are used for monitoring the hydrogen concentration that the sealed face of anchor clamps leaked.
The testing device and the testing method provided by the invention can systematically and accurately test the hydrogen permeability of different types of liner materials. Compared with the traditional test method, the method has the advantages that the test under constant test pressure can be realized, the test under circulating pressure can also be realized, the pressure measurement and temperature measurement range is wider, the functions are complete, the equipment integration level is high, and the like.
Drawings
Fig. 1 is a schematic structural diagram of a hydrogen permeability testing device provided by the invention.
Fig. 2 is a schematic view of the structure of the jig.
Description of reference numerals: a hydrogen cylinder group 1; a nitrogen gas cylinder group 2; a solenoid valve 3; a gas supply line 4; a one-way valve 5, a pressure sensor 6, a booster pump 7, a buffer tank 8, a cooler 9 and an air supply control valve 10; an air intake line 11; a jig 12; a shielding cover 13; a heat insulating cover 14; purging a nitrogen source 15; a purge valve 16; a manual valve 17; a pressure gauge 18; a temperature sensor 19; a heating power supply 20; a liquid nitrogen source 21; a cooling inlet pipe 22; a cooling-out pipe 23; a bypass line 24; a purge check valve 25; an inlet pipe control valve 26; an outlet pipe control valve 27; an air outlet channel 28; mass spectrometer number one 29; a mass spectrometer No. two 30; a signal numerical control device 31; a computer 32; an electric heating rod 33; a thermocouple 34; a cooling flow passage 35; a sample 36; a metal mesh 37; o- rings 38, 39.
Detailed Description
As shown in fig. 1 and 2, the invention provides a high-pressure hydrogen permeation test device for liner materials of an IV-type gas cylinder, which mainly comprises: the fixture 12 that the airtight sample that combines, the air supply system that is linked together with sample one side, the detecting system that is linked together with the sample opposite side and other parts to the gas environment of sample place supplementary control, wherein:
the gas supply system comprises a hydrogen cylinder group 1 and a nitrogen cylinder group 2, the hydrogen cylinder group 1 and the nitrogen cylinder group 2 are communicated with a gas supply pipeline 4 through a manual valve 17 and a gas supply electromagnetic valve 3 in a switching way, and the gas supply pipeline 4 is sequentially provided with a one-way valve 5, a pressure sensor 6, a booster pump 7, a buffer tank 8, a cooler 9, a gas supply control valve 10, an emptying valve 16, a pressure gauge 18 and a temperature sensor 19;
the clamp 12 is composed of an upper part and a lower part, the upper part and the lower part are fastened through bolts (not shown) to fix the sample 36, a pore passage communicated with one side of the sample 36 is arranged on the upper part of the clamp 12 and is connected with the air inlet pipeline 11 of the air supply system in a sealing way, a pore passage communicated with the other side of the sample 36 is arranged on the lower part of the clamp 12 and is communicated with the detection system, the sample 36 is connected with the clamp 12 in a sealing way through O- shaped sealing rings 38 and 39, and the pore passage on the upper part of the clamp 12 and the pore passage on the lower part of the clamp 12 are isolated by the sample 36; the sample 36 is a wafer sample 36 which is taken from an inner container of the gas cylinder, has the thickness of 2-5 mm and the diameter of 78mm, the test surface is cleaned, and burrs need to be removed at edges and corners;
an electric heating rod 33 is respectively fixed on the upper part of the clamp 12 and the lower part of the clamp 12, the electric heating rod 33 is connected to the heating power supply 20, and can heat the clamp 12 and the sample 36 clamped by the clamp; thermocouples 34 are respectively fixed on the upper part of the clamp 12 and the lower part of the clamp 12 and used for monitoring the temperature of the clamp 12; in addition, a cooling flow channel 35 is arranged at the upper part of the clamp 12 and/or at the inner part of the lower part of the clamp 12, the cooling flow channel 35 is communicated to a cooling working medium source (such as a liquid nitrogen source 21) through a cooling inlet pipe 22 and a cooling outlet pipe 23, and the temperature rise and/or the temperature drop are controlled by controlling the electric heating rod 33 and/or the cooling working medium, so that the temperature of the clamp 12 can be controlled within a preset range;
wherein, a cooling inlet pipe 22 is provided with an inlet pipe control valve 26, and a cooling outlet pipe 23 is provided with an outlet pipe control valve 27;
the detection system mainly comprises an air outlet channel 28 communicated with a pore canal at the lower part of the clamp 12, and the air outlet channel 28 is connected to a mass spectrometer 29;
an isolation cover 13 which hermetically surrounds the clamp 12 is arranged on the periphery of the clamp 12, a bypass pipeline 24 is opened on the isolation cover 13 and communicated with the isolation cover 13, the bypass pipeline 24 is divided into two paths, one path is connected to a second mass spectrometer 30, the other path is communicated to a purging nitrogen source 15 through a purging one-way valve 25, and the purging nitrogen source 15 can send purging nitrogen into the isolation cover 13 through the purging one-way valve 25;
a heat insulation cover 14 is arranged on the periphery of the isolation cover 13 to avoid or reduce the influence of the external environment temperature on the temperature of the clamp 12 and the temperature of the sample 36;
in addition, a signal numerical control device 31 is also arranged and is in signal connection with the mass spectrometer 29, the mass spectrometer 30 II, the gas supply electromagnetic valve 3, the pressure sensor 6, the booster pump 7, the gas supply control valve 10, the blow-down valve 16, the pressure gauge 18, the temperature sensor 19, the electric heating rod 33, the thermocouple 34, the pipe inlet control valve 26, the pipe outlet control valve 27 and the purging nitrogen source 15, and then is connected with a data processing device (such as a computer 32), so that the working process of the invention can be automatically controlled and monitored.
The hydrogen permeability test can be carried out by utilizing the device, and the hydrogen permeability test comprises the following steps of:
1. test method for hydrogen permeability test under constant pressure:
(1) sample 36 is prepared. The sample 36 is a round slice (thickness is 2-5 mm, diameter is 78mm) which is directly taken away from the inner container or is separately manufactured under the same processing condition, edge and burr is cleaned through surface cleaning treatment, the round slice is rapidly placed into a groove at the lower part of the clamp 12 after vacuum drying treatment, a sintered metal mesh 37 and an O-shaped sealing ring 38 are placed into the groove in advance, only the O-shaped sealing ring 39 is placed at the upper part of the clamp 12, then the upper part and the lower part of the clamp 12 are relatively fixed, and the upper surface and the lower surface of the sample 36 are respectively connected with the O- shaped sealing rings 38 and 39 in an airtight mode.
(2) And selecting heating and cooling functions. When a high-temperature environment test is carried out (Ttest is more than 20 ℃), an electric heating rod 33 is inserted into the side edge of the clamp 12, a cooling working medium source (such as a liquid nitrogen source 21) is disconnected, a stainless steel isolation cover 13 is covered, a bypass pipeline 24 on the isolation cover 13 is connected to a second mass spectrometer 30, and a heat insulation cover 14 is closed. A heating power supply 20 is switched on, the clamp 12 is heated to the test temperature through a heating rod 33, and then the temperature is kept for 30min to start air supply and detection;
when a low-temperature environment test is carried out (Ttest is less than or equal to 20 ℃), the heating rod 33 is taken out, a cooling working medium source (such as a liquid nitrogen source 21) is communicated, the stainless steel isolation cover 13 is covered and communicated with the second mass spectrometer 30, and the heat insulation cover 14 is closed. After the clamp 12 is cooled to the test temperature by controlling a cooling working medium source (such as a liquid nitrogen source 21), the temperature is kept for 30min, and gas supply and detection are started.
(3) The nitrogen gas is replaced in the shroud 13 and the inlet pipe 11. And after the test temperature reaches the standard, connecting a purging nitrogen source 15, opening an emptying valve 16 and a manual valve 17 of the nitrogen cylinder group 2, introducing nitrogen into the isolation cover 13 through a purging one-way valve 25, and performing nitrogen purging replacement on the air inlet pipeline 11 and the interior of the isolation cover 13 respectively, wherein the replacement pressure is 0.2-0.6 MPa.
(4) Constant pressurization and pressure maintaining. And (3) closing the air release valve 16 and the manual valve 17 of the nitrogen cylinder group 2, opening the hydrogen cylinder group 1, allowing hydrogen to enter the booster pump 7, controlling the booster pump 7 to be opened through the signal numerical control device 31, boosting the hydrogen, and allowing the high-pressure hydrogen to contact with the upper surface of the sample 36 through the air inlet pipeline 11 and the upper hole channel of the clamp 12 after the high-pressure hydrogen reaches the test pressure.
(5) And (5) detecting the concentration. After 5 minutes of holding pressure, hydrogen concentration detection was started. And simultaneously starting a mass spectrometer 29 and a mass spectrometer 30 for hydrogen monitoring, wherein the mass spectrometer 29 is used for monitoring hydrogen Q1 permeating in the thickness direction of the sample 36, and the mass spectrometer 30 is used for monitoring the hydrogen concentration Q2 leaked from the sealing surface of the clamp 12.
2. Hydrogen permeability test method at circulating pressure:
steps (1) to (3) are the same as in test method 1.
(4) And (4) pressure cycling. The method is characterized in that a software is set to be an automatic control circulation pressure mode, the upper limit of pressure is set to be not lower than 15MPa, the lower limit of pressure is set to be 5MPa, and the circulation frequency of hydrogen is set to be not higher than 2 minutes for 1 time. And (3) opening the hydrogen cylinder group 1, pressurizing hydrogen by a booster pump 7, then feeding the pressurized hydrogen into a buffer tank 8, contacting high-pressure hydrogen with the upper surface of a sample 36 through an air inlet pipeline 11 and a pore passage at the upper part of a clamp 12, maintaining the pressure for 10 seconds, closing an air supply control valve 10, slowly opening an air release valve 16 for releasing the pressure until the pressure is lower than 5MPa, closing the air release valve 16 for 3 seconds, and ending a pressure cycle. Immediately thereafter, the air supply control valve 10 is opened to perform the second pressure cycle.
(5) Hydrogen monitoring was performed simultaneously. The first mass spectrometer 29 is used for monitoring the hydrogen Q1 'permeating in the thickness direction of the sample 36, the second mass spectrometer 30 is used for monitoring the hydrogen concentration Q2' leaking from the sealing surface of the clamp 12, and the permeated hydrogen concentrations Q1 'and Q2' are recorded every 500 pressure cycles. And circulating for X times, and then calculating the total permeation quantity by the formula: Q-Q1' X/500.
Compared with the prior art, the invention has the beneficial effects that:
the testing device and the testing method provided by the invention can systematically and accurately test the hydrogen permeability of different types of liner materials. Compared with the traditional test method, the method has the advantages that the test under constant test pressure can be realized, the test under circulating pressure can also be realized, the pressure measurement and temperature measurement range is wider, the functions are complete, the equipment integration level is high, and the like.
Claims (10)
1. The utility model provides a high pressure hydrogen permeation test device of IV type gas cylinder inner bag material which characterized in that includes: the airtight anchor clamps that combine with the sample, the air supply system that is linked together and the detecting system that is linked together with the sample opposite side with sample one side, wherein:
the gas supply system comprises a gas supply pipeline communicated with the hydrogen cylinder group, the gas supply pipeline is connected to a gas inlet pipeline through a booster pump, and the gas inlet pipeline is closely communicated with one side surface of the sample;
the detection system comprises an air outlet pipeline which is closely connected and communicated with the other side surface of the sample, and the air outlet pipeline is connected to a mass spectrometer I.
2. The high-pressure hydrogen permeation test device for the liner material of the IV-type gas cylinder according to claim 1, which is characterized in that: and the periphery of the clamp is provided with a shielding cover which hermetically surrounds the clamp, the upper opening of the shielding cover is communicated with a bypass pipeline, and the bypass pipeline is connected to a second mass spectrometer.
3. The high-pressure hydrogen permeation test device for the liner material of the IV-type gas cylinder as claimed in claim 2, characterized in that: the gas supply pipeline is communicated with the hydrogen cylinder group and the nitrogen cylinder group in a switching mode, the bypass pipeline is communicated to a purging nitrogen source through a purging one-way valve, and the purging nitrogen source can send purging nitrogen into the isolation hood through the purging one-way valve.
4. The high-pressure hydrogen permeation test device for the liner material of the IV-type gas cylinder according to claim 3, characterized in that: and an air release valve is arranged on the air inlet pipeline.
5. The high-pressure hydrogen permeation test device for the liner material of the IV-type gas cylinder according to claim 4, characterized in that: and a buffer tank and an air supply control valve are sequentially arranged at the downstream of the booster pump of the air supply pipeline, and the air supply control valve is positioned at the upstream position of the emptying valve.
6. The high-pressure hydrogen permeation test device for the liner material of the IV-type gas cylinder according to claim 5, which is characterized in that: the upper part and the lower part of the clamp are respectively fixed with an electric heating rod which is connected to a heating power supply; and cooling channels are arranged in the upper part and/or the lower part of the clamp and communicated to the cooling working medium circulation pipeline.
7. The high-pressure hydrogen permeation test device for the liner material of the IV-type gas cylinder according to claim 6, which is characterized in that: and thermocouples are fixed on the upper part and/or the lower part of the clamp.
8. The high-pressure hydrogen permeation test device for the liner material of the IV-type gas cylinder according to claim 7, which is characterized in that: and the system is also provided with a signal numerical control device which is in signal connection with the mass spectrometer I, the mass spectrometer II, the booster pump, the air supply control valve, the blow-down valve, the electric heating rod, the thermocouple, the cooling working medium circulating pipeline and the purging nitrogen source and is connected with the data processing device.
9. A hydrogen permeability testing method under constant pressure, which uses the high-pressure hydrogen permeability testing device for the liner material of the IV-type gas cylinder as claimed in claim 8, and is characterized by comprising the following steps:
(1) sample preparation: placing a sample into a groove at the lower part of a clamp, placing a sintered metal mesh and an O-shaped sealing ring into the groove in advance, placing the O-shaped sealing ring at the upper part of the clamp, relatively fixing the upper part and the lower part of the clamp, and hermetically connecting the upper surface and the lower surface of the sample with the O-shaped sealing ring respectively;
(2) heating and cooling function selection:
when a high-temperature environment test is carried out, an electric heating rod is inserted into the side edge of the clamp, the cooling working medium circulation pipeline is disconnected, the isolation cover is covered, and a bypass pipeline on the isolation cover is connected to a second mass spectrometer; a heating power supply is switched on, and after the fixture is heated to the test temperature through the heating rod, the fixture is kept warm for a certain period of time;
when a low-temperature environment test is carried out, the heating rod is taken out, the heating rod is communicated with a cooling working medium circulation pipeline, the isolation cover is covered and communicated with a second mass spectrometer, and after the clamp is cooled to the test temperature through the cooling working medium circulation pipeline, the clamp is kept warm for a certain period of time;
(3) nitrogen replacement of the isolation cover and the air inlet pipeline: after the test temperature reaches the standard, connecting a purging nitrogen source, opening a vent valve, allowing nitrogen from the purging nitrogen source to enter the isolation hood through a purging one-way valve, and performing nitrogen purging replacement on the air inlet pipeline and the interior of the isolation hood respectively; meanwhile, the gas supply pipeline is switched to be communicated with the nitrogen cylinder group, so that the gas supply pipeline is replaced by nitrogen;
(4) constant pressurization and pressure maintaining: closing the air release valve, switching the air supply pipeline to be communicated with the hydrogen cylinder group, introducing hydrogen of the hydrogen cylinder group into the booster pump, and contacting the generated high-pressure hydrogen with the upper surface of the sample through the air inlet pipeline and the pore passage at the upper part of the clamp after the generated high-pressure hydrogen reaches the test pressure;
(5) and (3) detecting the hydrogen concentration: after maintaining the pressure for a period of time, starting hydrogen concentration detection: opening a mass spectrograph and No. two mass spectrometers simultaneously and carrying out the hydrogen monitoring, a mass spectrograph is used for monitoring the hydrogen of sample thickness direction infiltration, and No. two mass spectrometers are used for monitoring the hydrogen concentration of the sealed face leakage of anchor clamps.
10. A hydrogen permeability testing method under circulating pressure, which uses the high-pressure hydrogen permeability testing device for the liner material of the IV-type gas cylinder as claimed in claim 8, is characterized by comprising the following steps:
(1) sample preparation: placing a sample into a groove at the lower part of a clamp, placing a sintered metal mesh and an O-shaped sealing ring into the groove in advance, placing the O-shaped sealing ring at the upper part of the clamp, relatively fixing the upper part and the lower part of the clamp, and hermetically connecting the upper surface and the lower surface of the sample with the O-shaped sealing ring respectively;
(2) heating and cooling function selection:
when a high-temperature environment test is carried out, an electric heating rod is inserted into the side edge of the clamp, the cooling working medium circulation pipeline is disconnected, the isolation cover is covered, and a bypass pipeline on the isolation cover is connected to a second mass spectrometer; a heating power supply is switched on, and after the fixture is heated to the test temperature through the heating rod, the fixture is kept warm for a certain period of time;
when a low-temperature environment test is carried out, the heating rod is taken out, the heating rod is communicated with a cooling working medium circulation pipeline, the isolation cover is covered and communicated with a second mass spectrometer, and after the clamp is cooled to the test temperature through the cooling working medium circulation pipeline, the clamp is kept warm for a certain period of time;
(3) nitrogen replacement of the isolation cover and the air inlet pipeline: after the test temperature reaches the standard, connecting a purging nitrogen source, opening a vent valve, allowing nitrogen from the purging nitrogen source to enter the isolation hood through a purging one-way valve, and performing nitrogen purging replacement on the air inlet pipeline and the interior of the isolation hood respectively; meanwhile, the gas supply pipeline is switched to be communicated with the nitrogen cylinder group, so that the gas supply pipeline is replaced by nitrogen;
(4) pressure circulation: closing an air release valve, switching an air supply pipeline to be communicated with a hydrogen cylinder group, pressurizing hydrogen of the hydrogen cylinder group by a booster pump, then feeding the pressurized hydrogen into a buffer tank, enabling high-pressure hydrogen to be in contact with the upper surface of the sample through an air inlet pipeline and a hole channel at the upper part of the clamp, maintaining the pressure for several seconds, closing an air supply control valve, slowly opening the air release valve to release the pressure until the pressure is lower than a preset value, closing the air release valve, continuing for several seconds, and ending a pressure cycle; then opening the air supply control valve and continuously performing the next pressure cycle;
(5) hydrogen monitoring: a mass spectrometer and No. two mass spectrometers are opened simultaneously, and a mass spectrometer is used for monitoring the hydrogen of sample thickness direction infiltration, and No. two mass spectrometers are used for monitoring the hydrogen concentration that the sealed face of anchor clamps leaked.
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