CN116952782A - Device and method for testing hydrogen permeability of nonmetallic material - Google Patents
Device and method for testing hydrogen permeability of nonmetallic material Download PDFInfo
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 115
- 239000001257 hydrogen Substances 0.000 title claims abstract description 115
- 239000000463 material Substances 0.000 title claims abstract description 71
- 238000012360 testing method Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 50
- 230000035699 permeability Effects 0.000 title claims abstract description 19
- 239000007789 gas Substances 0.000 claims abstract description 229
- 230000007613 environmental effect Effects 0.000 claims abstract description 62
- 230000007246 mechanism Effects 0.000 claims abstract description 48
- 238000001514 detection method Methods 0.000 claims abstract description 26
- 238000012216 screening Methods 0.000 claims abstract description 8
- 239000003570 air Substances 0.000 claims description 177
- 238000002474 experimental method Methods 0.000 claims description 43
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 32
- 238000007789 sealing Methods 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000003860 storage Methods 0.000 claims description 20
- 239000003345 natural gas Substances 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- 230000008595 infiltration Effects 0.000 claims description 9
- 238000001764 infiltration Methods 0.000 claims description 9
- 239000012080 ambient air Substances 0.000 claims description 8
- 229910052755 nonmetal Inorganic materials 0.000 claims description 8
- 239000006260 foam Substances 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000007769 metal material Substances 0.000 claims description 5
- 238000011056 performance test Methods 0.000 claims description 5
- 238000005457 optimization Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000003749 cleanliness Effects 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000012795 verification Methods 0.000 claims description 3
- 238000011160 research Methods 0.000 abstract description 5
- 230000035515 penetration Effects 0.000 abstract description 3
- 230000003204 osmotic effect Effects 0.000 abstract description 2
- 238000011161 development Methods 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000003566 sealing material Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012611 container material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000009467 reduction 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
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/04—Investigating osmotic effects
-
- 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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- General Physics & Mathematics (AREA)
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Abstract
The invention provides a device and a method for testing hydrogen permeability of a nonmetallic material, wherein the device comprises the following components: the air source module consists of an experimental air source mechanism and an environmental air source mechanism, and provides a required osmotic air source and an environmental air source for the osmosis module through an air supply pipeline; the experimental gas module in the permeation module is connected with the experimental gas source mechanism through the experimental gas source connecting device, the environmental gas module is connected with the environmental gas source structure through the environmental gas source connecting device, and the experimental gas module and the environmental gas module form a sealed cavity after being assembled to accommodate a sample; and collecting the gas of the environmental gas module after the penetration test is finished through the detection module and obtaining an experimental result. The device is used for realizing the test, can overcome the test limitation of the prior art, dynamically reflects the hydrogen permeation characteristic of the nonmetallic material under the real working condition, and provides a reliable basis for the screening research of the nonmetallic material of hydrogen energy.
Description
Technical Field
The invention relates to the technical field of hydrogen energy safety operation, in particular to a device and a method for testing hydrogen permeability of a nonmetallic material.
Background
Hydrogen energy utilization is an effective way for realizing the ecological improvement green low-carbon optimization development target, and the industrial rapid introduction period is entered in a plurality of fields. High-pressure hydrogen storage systems operate in high-pressure and/or high-purity hydrogen environments for a long time, high-pressure hydrogen damage can occur, fracture risks caused by plastic loss, accelerated fatigue crack growth rate and durability reduction of functional materials of the system and high-pressure high-speed hydrogen impact are unavoidable, and hydrogen energy safety problems are common challenges facing related fields. Therefore, the hydrogen compatibility evaluation of the material becomes a first link of the development of high-pressure hydrogen system products.
The existing hydrogen compatibility experimental device in the research result is mainly designed for testing metal materials, but the trend of applying a polymer sealing material of a hydrogen storage system and an inner container material of an IV-type hydrogen storage bottle to the field of hydrogen storage and hydrogen energy engineering is present in the recent years, in addition, researchers also have the continuous exploration of planning and developing the future non-metal pipeline hydrogen transportation work, and the development of hydrogen energy sources puts forward higher requirements on the non-metal hydrogen compatibility.
However, at present, no device for reasonably realizing hydrogen permeation test aiming at nonmetal exists in the system, and especially, the dynamic data of hydrogen permeation rate of a polymer sealing material of a hydrogen storage system, a liner material of an IV-type hydrogen storage bottle, a hydrogen delivery (hydrogen-loading) nonmetallic pipeline material and the like under the operating condition are not known.
The information disclosed in the background section of the invention is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
In order to solve the problems, the invention provides a device for testing the hydrogen permeability of a nonmetallic material, which aims to effectively reduce the gas environment of the inner surface and the outer surface of a nonmetallic material sample under the actual operating condition and measure the hydrogen permeability of the nonmetallic material under the actual operating condition. In one embodiment, the apparatus comprises:
the air source module comprises an experiment air source mechanism and an environment air source mechanism, wherein the experiment air source mechanism and the environment air source mechanism both comprise air supply pipelines, and a permeation air source and an environment air source for testing requirements are provided for the permeation module through the air supply pipelines; the experiment air source mechanism further comprises an air outlet pipeline for exhausting air after the experiment is completed;
the infiltration module consists of an experimental gas module and an environmental gas module which are detachably connected, the experimental gas module is connected with the experimental gas source mechanism through an experimental gas source connecting device, the environmental gas module is connected with the environmental gas source structure through an environmental gas source connecting device, and the experimental gas module and the environmental gas module form a sealed cavity for fixing a nonmetallic material sample after assembly; the method comprises the steps of carrying out a first treatment on the surface of the
The detection module is connected between the permeation module and the detection analysis system and is used for collecting the gas of the environmental gas module after the permeation test is finished and obtaining an experimental result to be transmitted to the detection analysis system.
Preferably, in one embodiment, the gas source of the experiment gas source mechanism comprises a hydrogen gas source and a natural gas source, and booster pumps are arranged on gas supply pipelines between the gas source and the experiment gas module so as to control the pressure of the provided experiment gas according to experiment requirements;
the air source of the environment air source mechanism adopts a nitrogen air source, and a booster pump is arranged on an air supply pipeline between the air source and the environment air source module so as to control the pressure of the provided environment air according to experimental requirements.
As a further improvement of the present invention, in one embodiment, the air supply lines of the experimental air supply mechanism and the environmental air supply mechanism each comprise: the manual valve, the air supply control valve and the pressure sensor are used for controlling the on-off and the air quantity of air in the air supply process according to experimental requirements, dynamically monitoring the air pressure state and supporting the air pressure regulation.
On the other hand, in one embodiment, the air supply pipelines of the experiment air source mechanism and the environment air source mechanism comprise one-way valves, and the one-way valves are used for avoiding reverse flow of air supply in the experiment process.
Further, in an embodiment, the experimental gas connection device and the environmental gas connection device each include a plurality of openable gas source connection ports, which are used for connecting different gas sources or connecting a vacuum pump according to experimental requirements.
Specifically, in one embodiment, the experimental gas module and the environmental gas module are combined through a bolt structure, and through holes are formed between the air outlet of the experimental gas connecting device and the cavity where the air outlet of the environmental gas connecting device and the sample are located.
In a preferred embodiment, the infiltration module is configured to: the non-metal material sample is arranged between the experimental gas module and the environmental gas module in parallel, one side of the sample is fixedly and hermetically connected with the experimental gas module through a sealing ring, and the other side of the sample is connected with the environmental gas module through an O-shaped sealing ring and foam metal.
In another aspect of the improvement of the invention, in one embodiment, the environmental gas module and the experimental gas module form a sealing cavity for fixing the bearing sample to perform the penetration test through a convex-concave fit structure so as to ensure the sealing performance and the structural stability.
Further, in one embodiment, after the assembly of the environmental gas module and the experimental gas module is completed, the sealing ring is flatly pressed, so that the tightness of the environment inside the ring relative to the outside of the ring is ensured.
Based on the application aspect of the device in any one or more of the foregoing embodiments, the present invention further provides a method for testing hydrogen permeation performance of a nonmetallic material, where the method is applied to the device in any one or more of the foregoing embodiments, and the method includes:
the method comprises the steps of sample preparation, obtaining a sheet nonmetallic material sample according to the size of a sealing cavity of the testing device, and performing verification screening and optimization treatment from the aspects of surface smoothness, material uniformity and cleanliness;
the method comprises the steps of sample fixing, namely cleaning and drying a nonmetallic material sample meeting requirements, then installing the nonmetallic material sample in a groove of an experimental gas module, placing an O-shaped sealing ring on the lower side of the sample in the groove in advance, and then tightly connecting the experimental gas module with an environmental gas module to ensure the integral tightness of the device;
the air source preparation step, selecting an air source according to the air source type, the air source proportion and the air pressure of the experimental requirement, setting the states of a manual valve, an air supply control valve and a booster pump of an air supply pipeline in the experimental air source mechanism and the environment air source mechanism, and closing an inlet and an outlet which are irrelevant to air supply in the permeation module;
the permeability detection step, after the air supply reaches the set experiment requirement and the pressure maintaining requirement time, an air outlet of an ambient air module is opened to collect ambient air through a detection module, and experimental result data are obtained;
and (3) a gas leakage step, namely opening a gas outlet of the experimental gas module, and discharging the experimental gas.
Further, in one embodiment, in the gas source preparation step, the pressure state of the gas in the gas supply pipeline is monitored by the pressure sensor, so as to provide support for controlling the booster pump.
Based on other aspects of the method described in any one or more of the embodiments above, the present invention also provides a storage medium having stored thereon program code that can implement the method described in any one or more of the embodiments above.
Compared with the closest prior art, the invention has the following beneficial effects:
the invention provides a device and a method for testing hydrogen permeability of a nonmetallic material, wherein the device comprises the following components: the air source module consists of an experimental air source mechanism and an environmental air source mechanism, and provides a required osmotic air source and an environmental air source for the osmosis module through an air supply pipeline; the experimental gas module in the permeation module is connected with the experimental gas source mechanism through the experimental gas source connecting device, the environmental gas module is connected with the environmental gas source structure through the environmental gas source connecting device, and the experimental gas module and the environmental gas module form a sealed cavity after assembly to accommodate a sample. The device is used for realizing the test, the testing limitation of the prior art can be overcome, the gas source type and the pressure level can be flexibly set, the gas environment (gas composition and pressure) on the inner surface and the outer surface of the nonmetallic material sample under the actual operation working condition can be comprehensively reduced, the hydrogen permeation characteristic of the nonmetallic material under the actual working condition can be reflected, and the screening research of nonmetallic materials under different application scenes such as a hydrogen delivery (hydrogen-adding) pipeline, a hydrogen storage container and the like can be realized.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention, without limitation to the invention. In the drawings:
FIG. 1 is a schematic diagram of a device for testing hydrogen permeation performance of nonmetallic materials according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a permeation module structure of a hydrogen permeation performance test device of a nonmetallic material according to an embodiment of the present invention;
FIG. 3 is a schematic illustration showing a structure of a gas source connection device of a hydrogen permeation performance test device of a nonmetallic material according to an embodiment of the present invention;
FIG. 4 is a flow chart of a method for testing hydrogen permeation performance of a nonmetallic material according to another embodiment of the present invention;
reference numerals illustrate: a hydrogen cylinder group 1; a manual valve 2; a one-way valve 3; a booster pump 4; a gas supply control valve 5; a pressure sensor 6; a natural gas cylinder group 7; a manual valve 8; a one-way valve 9; a booster pump 10; a gas supply control valve 11; a pressure sensor 12; a flow control valve 13; a nitrogen cylinder group 14; a manual valve 15; a one-way valve 16; a booster pump 17; a gas supply control valve 18; a pressure sensor 19; a detection analysis system 20; a gas supply line 21; an outlet gas line 22; bolt holes 23; an air source connection means 24; an O-ring 25; sample 26; a foam metal 27; an ambient gas module 28; an experiment gas module 29; a gas inlet and outlet 30.
Detailed Description
The following will explain the embodiments of the present invention in detail with reference to the drawings and examples, so that the practitioner of the present invention can fully understand how to apply the technical means to solve the technical problems, achieve the implementation process of the technical effects, and implement the present invention according to the implementation process. It should be noted that, as long as no conflict is formed, each embodiment of the present invention and each feature of each embodiment may be combined with each other, and the formed technical solutions are all within the protection scope of the present invention.
Although a flowchart depicts operations as a sequential process, many of the operations can be performed in parallel, concurrently, or at the same time. The order of the operations may be rearranged. The process may be terminated when its operations are completed, but may have additional steps not included in the figures. The processes may correspond to methods, functions, procedures, subroutines, and the like.
The terms "first," "second," and the like may be used herein to describe various elements, but these elements should not be limited by these terms, and these terms are used merely to distinguish one element from another. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items. When an element is referred to as being "connected" or "coupled" to another element, it can be directly connected or coupled to the other element or intervening elements may be present.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used herein, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
Hydrogen energy is an effective way for realizing the aim of ecologically improving green low carbon, and enters the industrial rapid introduction period at home and abroad. The high-pressure hydrogen storage system works in a high-pressure and high-purity hydrogen environment for a long time, high-pressure hydrogen damage possibly occurs, plastic damage is reduced, fatigue crack growth rate is accelerated, durability is reduced, and fracture danger caused by high-pressure and high-speed hydrogen impact is reduced, so that the problem of hydrogen energy safety becomes a common challenge at home and abroad. Therefore, the hydrogen compatibility evaluation of the material is the first link of the development of high-pressure hydrogen system products.
The existing hydrogen compatibility experimental device is mainly designed aiming at metal materials, however, along with the wide application of polymer sealing materials of a hydrogen storage system and liner materials of an IV-type hydrogen storage bottle and the continuous exploration of the future non-metal pipeline hydrogen transportation work, the development of hydrogen energy sources puts forward higher requirements on the non-metal hydrogen compatibility.
At present, a plurality of testing methods for the hydrogen permeability of nonmetallic hydrogen permeability devices, in particular to testing methods for the hydrogen permeability of polymer sealing materials of hydrogen storage systems, liner materials of IV-type hydrogen storage bottles, hydrogen delivery (hydrogen-doped) nonmetallic pipeline materials and the like under the operating condition are not mature.
In order to perfect the technical blank, the invention provides the device and the method for testing the hydrogen permeability of the nonmetallic material, so that the device and the method for testing the hydrogen permeability of the nonmetallic material under different working conditions of a high-pressure hydrogen system can be used for providing guidance for nonmetallic material selection for a hydrogen storage container and a hydrogen delivery (hydrogen-loading) pipeline, and have extremely important significance.
The detailed design and connection structure of the test device according to the embodiment of the present invention are described in detail below based on the drawings. In which, while the principle and order of operation of the structures are illustrated in the functional description, in some cases, the operations illustrated or described may be performed in an order different from that herein.
Example 1
Fig. 1 is a schematic structural diagram of a device for testing hydrogen permeation performance of a nonmetallic material according to a first embodiment of the present invention, and referring to fig. 1, it can be known that the device includes:
the air source module comprises an experiment air source mechanism and an environment air source mechanism, wherein the experiment air source mechanism and the environment air source mechanism both comprise air supply pipelines, and a permeation air source and an environment air source for testing requirements are provided for the permeation module through the air supply pipelines; the experiment air source mechanism further comprises an air outlet pipeline for exhausting air after the experiment is completed;
the infiltration module consists of an experimental gas module and an environmental gas module which are detachably connected, the experimental gas module is connected with the experimental gas source mechanism through an experimental gas source connecting device, the environmental gas module is connected with the environmental gas source structure through an environmental gas source connecting device, and a sealing cavity for fixing a nonmetallic material sample is formed by a groove part of the assembled experimental gas module and a convex part of the environmental gas module;
and the detection module is connected between the permeation module and the detection analysis system and is used for collecting the gas of the environmental gas module after the hydrogen permeation test is finished and obtaining an experimental result to be transmitted to the detection analysis system.
The testing device provided by the embodiment of the invention can solve the problem of hydrogen permeation testing of the nonmetallic material, in particular to the method and the device for testing the hydrogen permeation of the nonmetallic material, which can reduce the gas environment (gas composition and pressure) of the inner surface and the outer surface of the nonmetallic material sample under the actual operation condition and reflect the hydrogen permeation characteristics of the nonmetallic material under the actual operation condition, thereby realizing screening research of the nonmetallic material under different application scenes such as a hydrogen delivery (hydrogen-adding) pipeline, a hydrogen storage container and the like.
Specifically, in one embodiment, the air source of the experiment air source mechanism comprises a hydrogen air source and a natural gas air source, and booster pumps are arranged on air supply pipelines between the air source and the experiment air module so as to control the pressure of the provided experiment air according to experiment requirements;
the air source of the environment air source mechanism adopts a nitrogen air source, and a booster pump is arranged on an air supply pipeline between the air source and the environment air source module so as to control the pressure of the provided environment air according to experimental requirements.
Further, in one embodiment, the air supply pipeline of the experiment air supply mechanism and the air supply pipeline of the environment air supply mechanism comprise: the manual valve, the air supply control valve and the pressure sensor are used for controlling the on-off and the air quantity of air in the air supply process according to experimental requirements, dynamically monitoring the air pressure state and supporting the air pressure regulation.
In a preferred embodiment, the air supply pipelines of the experiment air source mechanism and the environment air source mechanism comprise one-way valves, and the one-way valves are used for avoiding reverse flow of air supply in the experiment process.
In addition, in one embodiment, the experimental gas connecting device and the environmental gas connecting device each comprise a plurality of openable gas source connecting ports, which are used for connecting different gas sources or connecting a vacuum pump according to experimental requirements.
In one embodiment, the experimental gas module and the environmental gas module are combined through a bolt structure, and through holes are formed between the air outlet of the experimental gas connecting device and the cavity where the air outlet of the environmental gas connecting device and the sample are located.
Further, in one embodiment, the infiltration module is configured to: the non-metal material sample is arranged between the experimental gas module and the environmental gas module in parallel, one side of the sample is fixedly and hermetically connected with the experimental gas module through a sealing ring, and the other side of the sample is connected with the environmental gas module through an O-shaped sealing ring and foam metal.
As can be seen from the information in fig. 1, the non-metallic sample in the permeation module is in contact with the experimental gas on one side and the ambient gas on the other side. The experimental gas module and the environmental gas module are respectively provided with an air inlet pipeline and an air outlet pipeline,
the experiment gas module can select pure hydrogen as a gas source to perform hydrogen permeation test of the nonmetallic sample in a high-pressure hydrogen environment; and the hydrogen permeation test of the nonmetallic material in the hydrogen-doped natural gas environment can be performed by calculating and selecting the mixed gas of hydrogen and natural gas with different proportions as a gas source. The experimental gas pressure can reach the gas pressure requirement of the actual working condition through the booster pump.
In practical application, the ambient gas module can select a nitrogen source, the pressure is generally standard atmospheric pressure, and the pressure can also be adjusted according to special experimental requirements. The gas outlet of the ambient gas module is connected with the detection analysis system module through a detection module, and the detection module consists of a gas acquisition device, a mass spectrometer and the like.
The nonmetallic material hydrogen permeability testing device is characterized in that a check valve, a booster pump, a gas supply regulating valve and a pressure sensor (pressure gauge) are arranged on an air inlet pipeline of the gas supply system. And a flow control valve is arranged on an air outlet pipe of the experimental gas module.
As shown in fig. 2: the sample is fixed in the infiltration module by the sealing washer, and the infiltration module comprises upper portion ambient gas module and lower part experiment gas module, and both are by bolted connection. The environment gas module and the experiment gas module are both provided with a gas source connecting device for realizing gas inlet and outlet (as shown in figure 3), and the device comprises a plurality of gas source connecting ports, can be connected with different gas sources according to experiment needs and also can be connected with a vacuum pump (when the experiment needs vacuum conditions), and can be directly closed when not in use.
In a preferred embodiment, the environmental gas module and the experimental gas module are arranged to form a sealing cavity for fixing a bearing sample to perform a penetration test through a convex-concave fit structure, and the sealing cavity is different from a double-concave hollow structure in a conventional embodiment.
Further, in one embodiment, after the assembly of the environmental gas module and the experimental gas module is completed, the sealing ring in the cavity is flatly pressed, so that the tightness of the environment in the ring relative to the outside of the ring is ensured. When the test is executed, the test gas and the environmental gas in the sealing ring are sealed relative to the environment of other inner cavities, and the test device can be flexibly applied to nonmetallic material samples with different sizes and thicknesses, so that the effective permeability test is realized.
The device for testing the hydrogen permeability of the nonmetallic material provided by the embodiment of the invention comprises a gas source module, a permeation module (divided into an experimental gas module and an environmental gas module), a detection module and the like. The surface of one side of the nonmetallic sample in the infiltration module is contacted with experimental gas, and the other side of the sample is contacted with ambient gas. The experimental gas module and the environmental gas module are respectively provided with an air inlet pipeline and an air outlet pipeline, and the experimental gas module can select pure hydrogen as an air source to perform hydrogen permeation test of the nonmetallic sample in a high-pressure hydrogen environment; and the hydrogen permeation test of the nonmetallic material in the hydrogen-doped natural gas environment can be performed by calculating and selecting the mixed gas of hydrogen and natural gas with different proportions as a gas source. The experimental gas pressure can reach the gas pressure requirement of the actual working condition through the booster pump. The ambient gas module selects a nitrogen source, the pressure is generally standard atmospheric pressure, and the pressure can be regulated according to special experimental requirements. The air outlet pipeline of the ambient gas module is connected with a detection module, and the detection module consists of a gas acquisition device, a mass spectrometer and the like. The air source connecting device of the environment air module and the experimental air module comprises a plurality of air source connecting ports, different air sources can be connected according to experimental requirements, a vacuum pump can be connected, and the air source connecting device can be directly closed when not in use.
Specifically, in one embodiment, with reference to the structural information in fig. 1, the gas source module includes a hydrogen cylinder group 1, a natural gas cylinder group 2 and a nitrogen cylinder group 14, where the hydrogen cylinder group 1, the natural gas cylinder group 2 and the nitrogen cylinder group 14 are respectively communicated with a gas supply pipeline 21 through a manual valve 2, a manual valve 8 and a manual valve 15, a check valve 3, a booster pump 4, a gas supply control valve 5 and a pressure sensor 6 are sequentially arranged on the hydrogen gas supply pipeline, a check valve 9, a booster pump 10, a gas supply control valve 11 and a pressure sensor 12 are sequentially arranged on the natural gas supply pipeline, and a check valve 16, a booster pump 17, a gas supply control valve 18 and a pressure sensor 19 are sequentially arranged on the nitrogen gas supply pipeline.
Further, as shown in fig. 2, the permeation module is composed of an upper ambient gas module 28 and a lower experimental gas module 29, and the upper and lower parts are fastened by bolts (not shown) to fix the sample 26. The surrounding gas module 28 at the upper part of the permeation module is provided with a pore canal communicated with one side surface of the sample 26 and is in sealing connection with an air inlet pipeline of the nitrogen gas supply system; the experimental gas module 29 at the lower part of the permeation module is provided with a pore canal communicated with the other side of the sample 26 and is in sealing connection with a hydrogen gas supply system and an air inlet pipeline of the natural gas supply system; the sample 26 and the upper ambient gas module 28 and the lower test gas module 29 are sealed by an O-ring 25. The sample 26 is a nonmetallic material with the thickness of 2-5 mm and the diameter of 70mm in each application scene of hydrogen storage and hydrogen transportation.
The invention can reduce the gas environment (including gas components, pressure and the like) of the inner and outer surfaces of the nonmetallic material sample under the actual operation condition, reflect the hydrogen permeation characteristic of the nonmetallic material under the actual operation condition, and realize the nonmetallic material screening research under different application scenes such as a hydrogen delivery (hydrogen-doped) pipeline, a hydrogen storage container and the like. The method can be used for the screening and safety evaluation work of nonmetallic materials in the whole process industrial chain of hydrogen energy industry production, storage, transportation and addition, and has wide application prospect.
In the device for testing the hydrogen permeability of the nonmetallic material, provided by the embodiment of the invention, each module or unit structure can independently or in combination operate according to experimental requirements so as to realize corresponding technical effects.
Example two
The embodiment of the invention disclosed above describes the structure of the device in detail, and based on the application aspect of the device in any one or more embodiments, the invention also provides a method for testing the hydrogen permeation performance of the nonmetallic material, which is applied to the device for testing the hydrogen permeation performance of the nonmetallic material in any one or more embodiments. Specific examples are given below for details.
Specifically, fig. 4 shows a schematic flow chart of a method for testing hydrogen permeation performance of a nonmetallic material according to an embodiment of the present invention, and as shown in fig. 4, the method includes:
the method comprises the steps of sample preparation, obtaining a sheet nonmetallic material sample according to the size of a sealing cavity of the testing device, and performing verification screening and optimization treatment from the aspects of surface smoothness, material uniformity and cleanliness;
the method comprises the steps of sample fixing, namely cleaning and drying a nonmetallic material sample meeting requirements, then installing the nonmetallic material sample in a groove of an experimental gas module, arranging an O-shaped sealing ring on the lower side of the sample in the groove in advance, arranging the O-shaped sealing ring and foam metal on the upper side of the sample, and tightly connecting the experimental gas module and the environmental gas module through bolts to ensure the overall tightness of the device;
the air source preparation step, selecting an air source according to the air source type, the air source proportion and the air pressure of the experimental requirement, setting the states of a manual valve, an air supply control valve and a booster pump of an air supply pipeline in the experimental air source mechanism and the environment air source mechanism, and closing an inlet and an outlet which are irrelevant to air supply in the permeation module;
the permeability detection step, after the air supply reaches the set experiment requirement and the pressure maintaining requirement time, an air outlet of an ambient air module is opened to collect ambient air, and experimental result data is obtained through a detection module;
and (3) a gas leakage step, namely opening a gas outlet of the experimental gas module, and discharging the experimental gas.
Further, in one embodiment, in the gas source preparation step, the pressure state of the gas in the gas supply pipeline is monitored by the pressure sensor, so as to provide support for controlling the booster pump.
In practical application, when the nonmetallic material hydrogen permeation performance test device provided by the embodiment of the invention is used for carrying out experiments, the method mainly comprises the following steps:
sample 26 preparation: nonmetallic materials used in a high-pressure hydrogen environment are processed into round thin sheets (the thickness is 2-5 mm and the diameter is 70 mm), and the surfaces are cleaned to ensure smooth, uniform and defect-free surfaces, so that experimental errors caused by manufacturing defects are eliminated. After the sample is cleaned and dried, the sample is quickly arranged in a groove of an experimental gas module 29, an O-shaped sealing ring 25 is arranged in the groove in advance, and the O-shaped sealing ring 25 and foam metal 27 are arranged on the upper part of the sample 26; the experimental gas module 29 is tightly connected with the environmental gas module 28 through bolts, so that the tightness of the whole device is ensured;
(2) Experimental gas module 29 preparation: closing the manual valves and corresponding air inlets of other bottle groups, selecting the hydrogen bottle group 1 as an air source, opening the manual valve 2 of the hydrogen bottle group 1 to enable hydrogen to enter the booster pump 4, pressurizing the hydrogen to enable the pressure of the experimental gas module 29 to reach the experimental pressure, enabling the experimental gas module 29 to be in contact with the lower surface of the sample 26 through the air inlet pipeline 21, the air source connecting device 24 and the pore canal of the experimental gas module 29, and keeping pressure stably;
(3) The ambient gas module 28 prepares: the nitrogen cylinder group 14 is selected as an air source, other air inlets are closed, and a manual valve 15 of the nitrogen cylinder group 14 is opened to enable the pressure of the ambient air to reach the standard atmospheric pressure; the nitrogen contacts with the upper surface of the sample 26 through the air inlet pipeline 21, the air source connecting device 24 and the pore canal of the ambient air module 28, and can stably maintain pressure;
(4) Hydrogen concentration detection: after a period of dwell, the ambient gas module 28 is subjected to gas collection and hydrogen concentration detection analysis by the detection analysis system 20.
In another embodiment, the hydrogen cylinder group 1 and the natural gas cylinder group 2 are selected as air sources in the preparation process of the experimental gas module 29, the volume ratio of hydrogen and natural gas is calculated according to different hydrogen loading ratios required by experiments, the experimental gas module 29 is supplied with air through a hydrogen supply system and a natural gas supply system respectively, the pressure of the experimental gas module 29 reaches the experimental requirement through the booster pumps 4 and 10, and the hydrogen loading natural gas contacts with the lower surface of the sample 26 and can be stably maintained in pressure;
for the foregoing method embodiments, for simplicity of explanation, the methodologies are shown as a series of acts, but one of ordinary skill in the art will appreciate that the present invention is not limited by the order of acts, as some steps may, in accordance with the present invention, occur in other orders or concurrently. Further, those skilled in the art will also appreciate that the embodiments described in the specification are all preferred embodiments, and that the acts and modules referred to are not necessarily required for the present invention.
It should be noted that in other embodiments of the present invention, the method may also be used to obtain a new method for testing the hydrogen permeation performance of a nonmetallic material by combining one or more of the above embodiments, so as to implement a performance test analysis on the hydrogen energy material.
It should be noted that, based on the method in any one or more of the foregoing embodiments of the present invention, the present invention further provides a storage medium, where a program code capable of implementing the method in any one or more of the foregoing embodiments is stored, where the code is executed by an operating system, to implement the method for testing hydrogen permeation performance of a nonmetallic material as described above.
It is to be understood that the disclosed embodiments are not limited to the specific structures, process steps, or materials disclosed herein, but are intended to extend to equivalents of these features as would be understood by one of ordinary skill in the relevant arts. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments only, and is not intended to be limiting.
Reference in the specification to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. Thus, the appearances of the phrase "one embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment.
Although the embodiments of the present invention are described above, the embodiments are only used for facilitating understanding of the present invention, and are not intended to limit the present invention. Any person skilled in the art can make any modification and variation in form and detail without departing from the spirit and scope of the present disclosure, but the scope of the present disclosure is still subject to the scope of the appended claims.
Claims (12)
1. A hydrogen permeation performance test device of a nonmetallic material, characterized in that the device comprises:
the air source module comprises an experiment air source mechanism and an environment air source mechanism, wherein the experiment air source mechanism and the environment air source mechanism both comprise air supply pipelines, and a permeation air source and an environment air source for testing requirements are provided for the permeation module through the air supply pipelines; the experiment air source mechanism further comprises an air outlet pipeline for exhausting air after the experiment is completed;
the infiltration module consists of an experimental gas module and an environmental gas module which are detachably connected, the experimental gas module is connected with the experimental gas source mechanism through an experimental gas source connecting device, the environmental gas module is connected with the environmental gas source structure through an environmental gas source connecting device, and the experimental gas module and the environmental gas module form a sealed cavity for fixing a nonmetallic material sample after assembly;
the detection module is connected between the permeation module and the detection analysis system and is used for collecting the gas of the environmental gas module after the permeation test is finished and obtaining an experimental result to be transmitted to the detection analysis system.
2. The apparatus of claim 1, wherein the gas source of the experiment gas source mechanism comprises a hydrogen gas source and a natural gas source, and booster pumps are arranged on the gas supply pipelines between the gas source and the experiment gas module to control the pressure of the supplied experiment gas according to experiment requirements;
the air source of the environment air source mechanism adopts a nitrogen air source, and a booster pump is arranged on an air supply pipeline between the air source and the environment air source module so as to control the pressure of the provided environment air according to experimental requirements.
3. The apparatus of claim 1, wherein the experiment gas supply mechanism and the environmental gas supply mechanism each comprise: the manual valve, the air supply control valve and the pressure sensor are used for controlling the on-off and the air quantity of air in the air supply process according to experimental requirements, dynamically monitoring the air pressure state and supporting the air pressure regulation.
4. The apparatus of claim 1, wherein the air supply lines of the experiment air supply mechanism and the environment air supply mechanism each comprise a check valve for preventing reverse flow of air supply during the experiment.
5. The device according to claim 1, wherein the experimental gas connection device and the environmental gas connection device each comprise a plurality of openable gas source connection ports for connecting different gas sources or vacuum pumps according to experimental requirements.
6. The device according to claim 1, wherein the experimental gas module and the environmental gas module are combined through a bolt structure, and through holes are formed between the air outlet of the experimental gas connecting device and the cavity where the air outlet of the environmental gas connecting device and the sample are located.
7. The apparatus of claim 1, wherein the infiltration module is configured to: the non-metal material sample is arranged between the experimental gas module and the environmental gas module in parallel, one side of the sample is fixedly and hermetically connected with the experimental gas module through a sealing ring, and the other side of the sample is connected with the environmental gas module through an O-shaped sealing ring and foam metal.
8. The apparatus of claim 1, wherein the environmental gas module and the experimental gas module are configured to form a sealed cavity for fixing a load-bearing sample to perform a permeation test by a convex-concave fit structure so as to ensure sealing performance and structural stability.
9. The device of claim 1, wherein after the assembly of the environmental gas module and the experimental gas module is completed, the sealing ring is flatly compressed, so that the tightness of the environment inside the ring relative to the environment outside the ring is ensured.
10. A method for testing hydrogen permeation performance of a nonmetallic material, for use in the apparatus of any one of claims 1 to 9, comprising:
the method comprises the steps of sample preparation, obtaining a sheet nonmetallic material sample according to the size of a sealing cavity of the testing device, and performing verification screening and optimization treatment from the aspects of surface smoothness, material uniformity and cleanliness;
the method comprises the steps of sample fixing, namely cleaning and drying a nonmetallic material sample meeting requirements, then installing the nonmetallic material sample in a groove of an experimental gas module, placing an O-shaped sealing ring on the lower side of the sample in the groove in advance, and then tightly connecting the experimental gas module with an environmental gas module to ensure the integral tightness of the device;
the air source preparation step, selecting an air source according to the air source type, the air source proportion and the air pressure of the experimental requirement, setting the states of a manual valve, an air supply control valve and a booster pump of an air supply pipeline in the experimental air source mechanism and the environment air source mechanism, and closing an inlet and an outlet which are irrelevant to air supply in the permeation module;
the permeability detection step, after the air supply reaches the set experiment requirement and the pressure maintaining requirement time, an air outlet of an ambient air module is opened to collect ambient air through a detection module, and experimental result data are obtained;
and (3) a gas leakage step, namely opening a gas outlet of the experimental gas module, and discharging the experimental gas.
11. The method of claim 10, wherein in the gas source preparation step, the pressure state of the gas in the gas supply line is monitored by a pressure sensor to provide support for the control of the booster pump.
12. A storage medium having stored thereon program code for implementing the method of claim 10 or 11.
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| CN117169088A (en) * | 2023-11-03 | 2023-12-05 | 大连理工大学 | High-pressure hydrogen permeation continuous monitoring device and testing method thereof |
| CN117169088B (en) * | 2023-11-03 | 2024-01-09 | 大连理工大学 | High-pressure hydrogen permeation continuous monitoring device and testing method thereof |
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