CN117092010A - High-pressure hydrogen permeation test device and pressure difference test method for IV type gas cylinder liner material - Google Patents
High-pressure hydrogen permeation test device and pressure difference test method for IV type gas cylinder liner material Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 112
- 239000001257 hydrogen Substances 0.000 title claims abstract description 101
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 101
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 239000007789 gas Substances 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 title claims abstract description 44
- 238000010998 test method Methods 0.000 title claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 44
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- 238000010926 purge Methods 0.000 claims description 13
- 238000012544 monitoring process Methods 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 15
- 238000010276 construction Methods 0.000 abstract description 8
- 230000005587 bubbling Effects 0.000 abstract description 7
- 238000011056 performance test Methods 0.000 abstract description 3
- 239000000306 component Substances 0.000 description 21
- 239000002184 metal Substances 0.000 description 11
- 238000001514 detection method Methods 0.000 description 7
- 238000009792 diffusion process Methods 0.000 description 6
- 229920001903 high density polyethylene Polymers 0.000 description 6
- 238000007789 sealing Methods 0.000 description 5
- 230000035699 permeability Effects 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 239000008358 core component Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241000617482 Kiwa Species 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000036962 time dependent Effects 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
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
- G01N3/10—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces generated by pneumatic or hydraulic pressure
- G01N3/12—Pressure testing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
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Abstract
The invention provides a high-pressure hydrogen permeation test device and a pressure difference test method for an IV type gas cylinder liner material, which relate to the technical field of gas cylinder liner material performance tests. The invention also provides a high-pressure hydrogen permeation test method for the IV gas cylinder liner material, which is used for developing the high-pressure hydrogen permeation test of the IV gas cylinder liner material by a differential pressure method so as to reduce the test construction cost and can be used for researching the bubbling behavior of the liner material under different pressure release rates.
Description
Technical Field
The invention relates to the technical field of performance tests of gas cylinder liner materials, in particular to a high-pressure hydrogen permeation test device and a pressure difference test method for an IV gas cylinder liner material.
Background
In recent years, hydrogen fuel cell automobiles have been rapidly developed as a main application of hydrogen energy in the transportation field, and hydrogen storage cylinders have also been rapidly developed as one of the core components of hydrogen fuel cell automobiles. Currently, vehicle-mounted III-type hydrogen storage cylinders and IV-type hydrogen storage cylinder products with the pressure of 35MPa and 70MPa are mainly adopted. The IV type hydrogen storage cylinder has the advantages of light weight, good fatigue resistance, high quality hydrogen storage density, low cost and the like, and is concerned by the field of international hydrogen energy automobiles. The plastic liner is used as one of the core components of the hydrogen storage cylinder, and becomes a research hot spot worldwide. At present, nylon and high-density polyethylene are mainly selected as plastic liner materials at home and abroad. Under the high-pressure hydrogen environment, the polymer liner material can generate hydrogen permeation behavior, and the liner can be damaged by buckling, bubbling and the like after the rapid pressure relief. In addition, hydrogen accumulation occurs when the vehicle is parked in a relatively airtight space for a long period of time, increasing the risk of fire explosion. Therefore, the hydrogen permeability of the liner material in a high-pressure environment is a key index for selecting the liner material and is also an important index for safely using the hydrogen storage cylinder with the plastic liner. The hydrogen permeation test device is used for developing the high-pressure hydrogen permeation performance test of the liner material, and is a key technical means for gas cylinder development. At present, hydrogen permeation test devices for plastic liner materials are developed in the United states, japan and European countries, for example, carrier gas hydrogen permeation test devices with test pressure reaching 90MPa are developed in Japanese university, and KIWA company and TESTNET company also develop hydrogen permeation test devices for plastic liner materials with working pressure of 20-90MPa successively, so that the hydrogen permeation related coefficient test of the liner materials is realized. Through investigation, the control of the pressure release rate of the hydrogen permeation test is not mentioned by the existing device, and the hydrogen permeation coefficient of the material is calculated by mostly measuring the volume or concentration of permeated hydrogen through a carrier gas method, so that the device for measuring the hydrogen permeation coefficient by the carrier gas method has high construction cost, and a novel scheme is urgently needed to solve the problems.
Disclosure of Invention
The invention aims to provide a high-pressure hydrogen permeation test device and a pressure difference test method for an IV type gas cylinder liner material, so as to solve the problems in the prior art, and the pressure difference method is used for developing the high-pressure hydrogen permeation test of the IV type gas cylinder liner material so as to reduce the test construction cost and conduct bubbling behavior research of the liner material under different pressure release rates.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides a high-pressure hydrogen permeation test device for IV gas cylinder liner materials, which comprises a low-pressure cavity, a high-pressure cavity, a vacuum gauge, a high-pressure hydrogen filling system and a pressure relief system, wherein a test sample is arranged between the low-pressure cavity and the high-pressure cavity, the test sample is isolated from the low-pressure cavity and the high-pressure cavity, the high-pressure hydrogen filling system is used for filling hydrogen into the high-pressure cavity, the vacuum gauge is used for monitoring the vacuum degree of the low-pressure cavity, the pressure relief system is communicated with the high-pressure cavity, and the opening degree of a pressure relief valve of the pressure relief system can be adjusted to realize pressure relief at different rates.
Preferably, a rigid support body is arranged between the test sample and the low-pressure cavity, and a plurality of holes are formed in the rigid support body to enable the surface of the test sample to be communicated with the low-pressure cavity.
Preferably, the low-pressure cavity is disposed in the upper component and extends to the lower surface of the upper component, the high-pressure cavity is disposed in the lower component and extends to the upper surface of the lower component, the upper component and the lower component are sandwiched by each other, and the upper surface and the lower surface of the test sample close to the outer edge are sealed with the gap between the upper component and the lower component.
Preferably, a plurality of annular supporting gaskets are arranged between the test sample and the lower assembly, and the number of the supporting gaskets is adjusted according to the thickness of the test sample so as to achieve the purpose of stably clamping the test sample.
Preferably, screw holes or through holes penetrating through the thickness direction are formed in the upper and lower assemblies so as to fix the upper and lower assemblies by screws and nuts.
Preferably, the upper assembly and the lower assembly are arranged in a constant temperature and humidity environment box, and the constant temperature and humidity environment box is communicated with an explosion-proof fan and a nitrogen generator.
Preferably, the pressure relief system comprises a rate control pressure relief passage, a conventional pressure relief passage and a standby pressure relief passage, wherein an electric proportional valve is added on the rate control pressure relief passage to control the opening of the pneumatic valve; the conventional pressure relief passage is used for non-timing normal pressure relief of the high-pressure side; the standby pressure relief passage is used for accident safety pressure relief.
Preferably, the device further comprises a nitrogen purging system, wherein the nitrogen purging system is used for purging the high-pressure cavity with nitrogen.
Preferably, the pressure relief system is communicated with the hydrogen recovery system.
The invention also provides a high-pressure hydrogen permeation test method for the IV gas cylinder liner material, which comprises the following steps:
step one, installing a tool and enabling a test sample to be located between a low-pressure cavity and a high-pressure cavity;
step two, adopting a constant temperature and humidity environment box to adjust the experimental environment;
step three, carrying out nitrogen purging on the high-pressure cavity, and then carrying out low-pressure hydrogen replacement to ensure that the oxygen content and the water content in the test system are respectively smaller than or equal to 1 multiplied by 10 -6 And 5X 10 -6 Stopping gas displacement when the gas is in a certain state;
step four, vacuumizing the low-pressure cavity by using a vacuum pump;
filling hydrogen with specified test pressure into the high-pressure cavity, and ensuring that a constant pressure difference is formed at two sides of the sample;
and step six, monitoring, processing and recording the pressure in the low-pressure cavity by a vacuum gauge, and stopping the test after the pressure increase rate of the low-pressure cavity is stabilized for 24 hours.
Compared with the prior art, the invention has the following technical effects:
according to the high-pressure hydrogen permeation test device for the IV gas cylinder liner material, provided by the invention, the pressure of gas in the low-pressure cavity is detected by using a vacuum gauge through a differential pressure method, the hydrogen permeation coefficient of a test sample is calculated according to a calculation formula, a pressure release system is arranged for the high-pressure cavity, and the opening of a pressure release valve of the pressure release system can be adjusted to realize pressure release at different rates. Therefore, the device provided by the invention can reduce the test construction cost and can be used for researching the bubbling behavior of the liner material under different pressure release rates.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a high-pressure hydrogen permeation test device for an IV gas cylinder liner material according to a first embodiment;
FIG. 2 is a schematic structural diagram of a hydrogen permeation tool;
in the figure: 1-a nitrogen cylinder group; 2-hydrogen cylinder group; 3-a gas molecular filter; 4-a manual valve; 5-a pressure sensor; 6-a pressure gauge; 7-an electromagnetic pneumatic valve; 8-a booster pump; 9-a buffer tank; a 10-cooler; 11-an electrical proportional valve; 12-a hydrogen recovery system; 13-an air inlet pipeline; 14-a constant temperature and humidity environment box; 15-an explosion-proof fan; 16-an electromagnetic valve; 17-a nitrogen making machine; 18-hydrogen permeation tooling; 19-hydrogen concentration monitor; 20-an air outlet pipeline; 21-an explosion-proof camera; 22-a pressure sensor 0-1MPa; 23-pressure sensor 0-500kPa; 24-vacuum gauge; 25-a vacuum pump; 26-bolts; 27-an intake passage; 28-a lower assembly; 29-upper assembly; 30-detection channel; 31-O type sealing ring; 32-sintering a metal support; 33-metal screen; 34-test specimen; 35-a support pad; 36-low pressure cavity.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention aims to provide a high-pressure hydrogen permeation test device and a pressure difference test method for an IV type gas cylinder liner material, so as to solve the problems in the prior art, and the pressure difference method is used for developing the high-pressure hydrogen permeation test of the IV type gas cylinder liner material so as to reduce the test construction cost and conduct bubbling behavior research of the liner material under different pressure release rates.
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to the appended drawings and appended detailed description.
Example 1
The embodiment provides a high-pressure hydrogen permeation test device for IV-type gas cylinder liner materials, as shown in fig. 1-2, the high-pressure hydrogen permeation test device comprises a low-pressure cavity 36, a high-pressure cavity, a vacuum gauge 24, a high-pressure hydrogen filling system and a pressure relief system, wherein a test sample 34 is arranged between the low-pressure cavity 36 and the high-pressure cavity, the test sample 34 isolates the low-pressure cavity 36 and the high-pressure cavity, the high-pressure hydrogen filling system is used for filling hydrogen into the high-pressure cavity, the vacuum gauge 24 is used for monitoring the vacuum degree of the low-pressure cavity 36, the pressure relief system is communicated with the high-pressure cavity, and the opening degree of a pressure relief valve of the pressure relief system is adjustable to realize pressure relief at different rates.
In the test, the permeation process of hydrogen gas in the test sample 34 can be understood as a diffusion process of hydrogen molecules from a high concentration to a low concentration in the test sample 34. High-pressure hydrogen is conveyed into the high-pressure cavity through a pipeline, permeates along the thickness direction of the test sample 34, and is detected, analyzed and calculated on the low-pressure cavity side through the vacuum gauge 24 to obtain the hydrogen permeation coefficient.
The high-pressure hydrogen permeation test device for the IV gas cylinder liner material provided by the embodiment only needs to be provided with the low-pressure cavity 36, the high-pressure cavity, the vacuum gauge 24, the high-pressure hydrogen filling system and the pressure relief system, and when the permeation coefficient test under constant pressure is carried out, the low-pressure cavity 36 and the high-pressure cavity are in a sealing state after the test is started, so that hydrogen in the high-pressure cavity can permeate into the low-pressure cavity 36 only through the test sample 34; when the bubbling behavior of the liner material under different pressure relief rates is detected, the pressure relief system needs to be opened and the opening of the pressure relief valve is adjusted to perform the test under different pressure relief rates.
Before the test, the high-pressure cavity needs to be purged with nitrogen and then replaced with hydrogen to remove air and moisture in the high-pressure cavity, and the low-pressure cavity 36 needs to be vacuumized, so that a nitrogen purging system is further needed, and the nitrogen purging system is used for purging the high-pressure cavity with nitrogen.
In order to reduce the test construction cost, the embodiment detects the gas pressure in the low-pressure cavity 36 by using a pressure difference method through the vacuum gauge 24, calculates the hydrogen permeability coefficient of the test sample 34 according to a calculation formula, and sets a pressure relief system for the high-pressure cavity, wherein the opening of a pressure relief valve of the pressure relief system can be adjusted to realize pressure relief at different rates. Therefore, the device provided by the invention can reduce the test construction cost and can be used for researching the bubbling behavior of the liner material under different pressure release rates.
The low pressure cavity 36 and the high pressure cavity are arranged in various ways, in order to facilitate the construction of the test, in some embodiments, the low pressure cavity 36 is arranged in the upper component 29 and extends to the lower surface of the upper component 29, the high pressure cavity is arranged in the lower component 28 and extends to the upper surface of the lower component 28, the test sample 34 is sandwiched between the upper component 29 and the lower component 28, and the upper surface and the lower surface of the test sample 34 close to the outer edge are sealed with the gap between the upper component 29 and the lower component 28, specifically, the O-ring 31 may be used to seal, that is, the O-ring 31 is arranged on the upper surface and the lower surface of the test sample 34 to avoid the gas in the low pressure cavity 36 and the high pressure cavity from leaking from the gap between the test sample 34 and the upper component 29 and the lower component 28.
The lower component 28 is provided with an air inlet channel 27, one end of the air inlet channel 27 is connected with the air inlet pipeline 13 of the high-pressure hydrogen filling system, the other end of the air inlet channel 27 is communicated with the high-pressure cavity, and part of the air inlet channel 27 at the tail end can be used as the high-pressure cavity, and the cross section of the high-pressure cavity is the same as that of the air inlet channel 27.
The upper assembly 29 is provided with a detection channel 30, one end of the detection channel 30 is communicated with the vacuum gauge 24 and the vacuum pump 25, and the other end is communicated with the low-pressure cavity 36. The detection channel 30 is also communicated with a pressure sensor 0-1MPa (22) and a pressure sensor 0-500kPa (23) so as to realize vacuumizing the low-pressure cavity 36 in a split-level vacuumizing mode, and the specific operation mode is as follows: the low pressure chamber is first pre-evacuated by vacuum pump 25 and then secondarily evacuated after maintaining the pressure for 30 minutes. When the prescribed vacuum is reached, the valve is closed.
In order to achieve the purpose of compressing the test sample 34 and the O-ring 31, the upper assembly 29 and the lower assembly 28 may be connected by a screw and a nut, specifically, screw holes or through holes penetrating through the thickness direction are formed in the upper assembly 29 and the lower assembly 28 to fix the upper assembly 29 and the lower assembly 28 by the screw and the nut, the screw sequentially passes through the upper assembly 29 and the lower assembly 28, the nuts are screwed at both ends of the screw, and the compression degree of the upper assembly 29 and the lower assembly 28 to the test sample 34 and the O-ring 31 is adjusted by adjusting the screwing degree of the nuts. Before the O-shaped sealing ring 31 is installed, vacuum sealing grease is uniformly smeared on the surface of the O-shaped sealing ring 31.
In addition, the purpose of connecting the upper assembly 29 and the lower assembly 28 may be achieved by a long bolt and a nut.
A plurality of screw holes or vias are provided in both the upper assembly 29 and the lower assembly 28.
In some embodiments, a passageway may be provided outside O-ring seal 31 and equipped with a hydrogen concentration monitor 19 for leak side monitoring and detection.
In some embodiments, to prevent the test specimen 34 from deforming toward the low pressure cavity 36 under high pressure differential, this embodiment provides a rigid support between the test specimen 34 and the low pressure cavity 36, and to provide a plurality of holes in the rigid support to allow the surface of the test specimen 34 to communicate with the low pressure cavity 36 so as not to impede hydrogen permeation. Specifically, the rigid support body may comprise a two-layer structure, wherein a metal screen 33 is arranged between the sintered metal support pieces 32, the metal screen 33 is arranged between the sintered metal support pieces 32 and the test sample 34, the mesh size of the metal screen 33 is less than or equal to 0.15mm, and the mesh area percentage is more than or equal to 35%. The sintered metal support 32 is used for supporting the test specimen 34 and the metal screen 33, and the aperture ratio of the sintered metal support 32 is not less than 40%.
In some embodiments, in order to meet the requirement that one fixture is used for testing test samples 34 with different thicknesses, the embodiment further includes a plurality of annular support gaskets 35, the support gaskets 35 are metal sheets, a plurality of annular support gaskets 35 can be arranged between the test samples 34 and the lower assembly 28, and the number of the support gaskets 35 is adjusted according to the thickness of the test samples 34 so as to achieve the purpose of stably clamping the test samples 34.
The bottom of the upper assembly 29 is provided with mounting locations for mounting rigid supports and the top surface of the lower assembly 28 is provided with mounting locations for mounting support pads 35.
The pressure relief system in the conventional scheme only comprises a rate control pressure relief passage, but in order to improve safety and convenience, the pressure relief system provided by the embodiment comprises a rate control pressure relief passage, a conventional pressure relief passage and a standby pressure relief passage, and an electric proportional valve 11 is added on the rate control pressure relief passage to control the opening of the pneumatic valve; the conventional pressure relief passage is used for non-timing normal pressure relief of the high-pressure side; the standby pressure relief passage is used for accident safety pressure relief.
In some embodiments, in order to achieve the purpose of accurately controlling the test environment, in this embodiment, the upper component 29 and the lower component 28 are disposed in a constant temperature and humidity environment box 14, and the constant temperature and humidity environment box 14 is communicated with an explosion-proof fan 15 and a nitrogen generator 17, so as to ensure that the hydrogen concentration in the environment box is sufficiently low, and the test operation is sufficiently safe. If the hydrogen concentration in the environment box is too high in the test process, the hydrogen concentration detection alarm device is started, and meanwhile, the explosion-proof fan 15 in the air conditioning channel is automatically associated and started, and nitrogen charging protection is carried out, so that the hydrogen concentration in the environment box is controlled at the lowest point.
An explosion-proof camera 21 can also be arranged in the constant temperature and humidity environment box 14 to record and record the image information therein.
In some embodiments, in order to save energy, the pressure relief system in this embodiment is connected to the hydrogen recovery system 12, and when the pressure relief system is used to relieve pressure of the hydrogen in the high-pressure cavity, the hydrogen can be discharged into the hydrogen recovery system 12 for storage and recycling.
In the above embodiment, the vacuum gauge 24 is used to monitor the pressure in the low-pressure cavity 36 in real time, so as to obtain the time-dependent pressure change curve of the low-pressure cavity 36 in the whole permeation process. The hydrogen permeability coefficient of the test specimen 34 can be calculated from the following formula:
wherein: p (P) e To test the gas permeability coefficient of sample 34, cm 3 ·cm/(cm 2 s.Pa); Δp/Δt is the arithmetic average value of the gas pressure change of the low-pressure cavity in unit time during stable permeation, pa/h; v is the volume of the low-pressure chamber, cm 3 The method comprises the steps of carrying out a first treatment on the surface of the s is the test area of the sample, cm 2 The method comprises the steps of carrying out a first treatment on the surface of the T is the test temperature, K; p is p 1 -p 2 The pressure difference Pa of the two sides of the sample; t (T) 0 、p 0 Temperature (273.15K) and pressure (1.0133 ×10) under standard conditions, respectively 5 Pa); d is the sample thickness, cm.
The diffusion coefficient of the gas in the test specimen 34 is determined according to the time-lag method, also known as the "high vacuum method", i.e. by calculating the diffusion coefficient D for the "lag time" when equilibrium is reached under high vacuum, by the formula:
wherein: l is the thickness of the sample, cm; θ is the lag time, s; d is diffusion coefficient cm 2 /s。
P e The product of the diffusion coefficient D and the solubility coefficient S, so that the solubility coefficient of the gas in the test sample 34 can be calculated by the formula in cm 3 /(cm 2 ·s·cm·Hg)。
Example two
The embodiment provides a high-pressure hydrogen permeation test method for an IV gas cylinder liner material, which comprises the following steps:
step one, installing a tool and enabling a test sample 34 to be located between a low-pressure cavity 36 and a high-pressure cavity; the volume of the low pressure chamber is known and the penetration area of the test specimen 34 is also known.
Step two, adopting a constant temperature and humidity environment box 14 to adjust the experimental environment; and after the heat preservation and moisture preservation are carried out for 1 hour, starting air supply and detection.
Step three, carrying out nitrogen purging on the high-pressure cavity, and then carrying out low-pressure hydrogen replacement to ensure that the oxygen content and the water content in the test system are respectively smaller than or equal to 1 multiplied by 10 -6 And 5X 10 -6 The gas displacement is stopped.
Step four, vacuumizing the low-pressure cavity 36 by using a vacuum pump 25; the low pressure chamber is first pre-evacuated by vacuum pump 25 and then secondarily evacuated after maintaining the pressure for 30 minutes. When the prescribed vacuum is reached, the valve is closed.
Specifically, a nitrogen purging source is connected, a nitrogen bottle manual valve and a vent valve are opened, nitrogen purging is carried out on a high-pressure pipeline and a high-pressure cavity, low-pressure hydrogen is selected for replacement, the replacement pressure is 0.2-0.6MPa, and the oxygen content and the water content in a system to be tested are respectively less than or equal to 1 multiplied by 10 -6 And 5X 10 -6 When the gas replacement is stopped and the nitrogen cylinder manual valve and the vent valve are closed.
Filling hydrogen with specified test pressure into the high-pressure cavity, and ensuring that a constant pressure difference is formed at two sides of the sample;
and step six, monitoring, processing and recording the pressure in the low-pressure cavity 36 through the vacuum gauge 24, and stopping the test after the pressure increase rate of the low-pressure cavity is stabilized for 24 hours.
The hydrogen permeation coefficient, diffusion coefficient, and solubility coefficient of the sample under test are obtained by analyzing the change in pressure in the low pressure chamber 36, and each coefficient can be found according to a standard.
The principles and embodiments of the present invention have been described in detail with reference to specific examples, which are provided to facilitate understanding of the method and core ideas of the present invention; also, it is within the scope of the present invention to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the invention.
Claims (10)
1. An IV type gas cylinder inner bag material high pressure hydrogen permeation test device, its characterized in that: including low pressure cavity, high pressure cavity, vacuum gauge, high pressure hydrogen filling system and pressure release system, the low pressure cavity with be used for setting up test sample between the high pressure cavity, test sample is isolated the low pressure cavity with the high pressure cavity, high pressure hydrogen filling system is used for to fill hydrogen in the high pressure cavity, the vacuum gauge is used for monitoring the vacuum degree of low pressure cavity, pressure release system intercommunication the high pressure cavity, just the aperture of pressure release valve of pressure release system is adjustable in order to realize the pressure release of different speed.
2. The high-pressure hydrogen permeation testing device for an IV gas cylinder liner material according to claim 1, wherein the high-pressure hydrogen permeation testing device comprises: and a rigid support body is arranged between the test sample and the low-pressure cavity, and a plurality of holes are formed in the rigid support body so that the surface of the test sample is communicated with the low-pressure cavity.
3. The high-pressure hydrogen permeation testing device for an IV gas cylinder liner material according to claim 2, wherein: the low-pressure cavity is arranged in the upper assembly and extends to the lower surface of the upper assembly, the high-pressure cavity is arranged in the lower assembly and extends to the upper surface of the lower assembly, the upper assembly and the lower assembly are used for clamping the test sample, and the upper surface and the lower surface of the test sample close to the outer edge are sealed with a gap between the upper assembly and the lower assembly.
4. The high-pressure hydrogen permeation testing device for an IV gas cylinder liner material according to claim 3, wherein: a plurality of annular supporting gaskets are arranged between the test sample and the lower assembly, and the number of the supporting gaskets is adjusted according to the thickness of the test sample so as to achieve the purpose of stably clamping the test sample.
5. The high-pressure hydrogen permeation testing device for an IV gas cylinder liner material according to claim 3, wherein: screw holes or through holes penetrating through the thickness direction are formed in the upper assembly and the lower assembly so as to fix the upper assembly and the lower assembly through screws and nuts.
6. The high-pressure hydrogen permeation testing device for an IV gas cylinder liner material according to claim 3, wherein: the upper assembly and the lower assembly are arranged in a constant temperature and humidity environment box, and the constant temperature and humidity environment box is communicated with an explosion-proof fan and a nitrogen generator.
7. The high-pressure hydrogen permeation testing device for an IV gas cylinder liner material according to claim 1, wherein the high-pressure hydrogen permeation testing device comprises: the pressure relief system comprises a rate control pressure relief passage, a conventional pressure relief passage and a standby pressure relief passage, wherein an electric proportional valve is added on the rate control pressure relief passage to control the opening of the pneumatic valve; the conventional pressure relief passage is used for non-timing normal pressure relief of the high-pressure side; the standby pressure relief passage is used for accident safety pressure relief.
8. The high-pressure hydrogen permeation testing device for an IV gas cylinder liner material according to claim 1, wherein the high-pressure hydrogen permeation testing device comprises: the nitrogen purging system is used for purging the high-pressure cavity with nitrogen.
9. The high-pressure hydrogen permeation testing device for an IV gas cylinder liner material according to claim 1, wherein the high-pressure hydrogen permeation testing device comprises: the pressure relief system is communicated with the hydrogen recovery system.
10. A high-pressure hydrogen permeation test method for IV-type gas cylinder liner materials is characterized by comprising the following steps of: comprising the following steps:
step one, installing a tool and enabling a test sample to be located between a low-pressure cavity and a high-pressure cavity;
step two, adopting a constant temperature and humidity environment box to adjust the experimental environment;
step three, carrying out nitrogen purging on the high-pressure cavity, and then carrying out low-pressure hydrogen replacement to ensure that the oxygen content and the water content in the test system are respectively smaller than or equal to 1 multiplied by 10 -6 And 5X 10 -6 Stopping gas displacement when the gas is in a certain state;
step four, vacuumizing the low-pressure cavity by using a vacuum pump;
filling hydrogen with specified test pressure into the high-pressure cavity, and ensuring that a constant pressure difference is formed at two sides of the sample;
and step six, monitoring, processing and recording the pressure in the low-pressure cavity by a vacuum gauge, and stopping the test after the pressure increase rate of the low-pressure cavity is stabilized for 24 hours.
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