CN115420665A - Device and method for measuring permeability of PE (polyethylene) pipe material under hydrogen-mixed natural gas - Google Patents
Device and method for measuring permeability of PE (polyethylene) pipe material under hydrogen-mixed natural gas Download PDFInfo
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- CN115420665A CN115420665A CN202211106535.8A CN202211106535A CN115420665A CN 115420665 A CN115420665 A CN 115420665A CN 202211106535 A CN202211106535 A CN 202211106535A CN 115420665 A CN115420665 A CN 115420665A
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000000463 material Substances 0.000 title claims abstract description 50
- 230000035699 permeability Effects 0.000 title claims abstract description 35
- 239000003345 natural gas Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000004698 Polyethylene Substances 0.000 title abstract description 55
- -1 polyethylene Polymers 0.000 title abstract description 6
- 229920000573 polyethylene Polymers 0.000 title abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 90
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 49
- 239000001257 hydrogen Substances 0.000 claims abstract description 49
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 42
- 239000010935 stainless steel Substances 0.000 claims abstract description 42
- 238000001764 infiltration Methods 0.000 claims abstract description 25
- 230000008595 infiltration Effects 0.000 claims abstract description 25
- 238000005057 refrigeration Methods 0.000 claims abstract description 14
- 238000012360 testing method Methods 0.000 claims description 25
- 239000003507 refrigerant Substances 0.000 claims description 19
- 238000011144 upstream manufacturing Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 11
- 238000011084 recovery Methods 0.000 claims description 10
- 230000002457 bidirectional effect Effects 0.000 claims description 9
- 239000003990 capacitor Substances 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000004888 barrier function Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000009792 diffusion process Methods 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 4
- 239000003381 stabilizer Substances 0.000 claims description 4
- 239000002826 coolant Substances 0.000 claims description 3
- 230000001960 triggered effect Effects 0.000 claims description 3
- 239000013526 supercooled liquid Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 claims 5
- 238000001035 drying Methods 0.000 claims 2
- 230000003584 silencer Effects 0.000 claims 1
- 239000010409 thin film Substances 0.000 claims 1
- 238000002474 experimental method Methods 0.000 abstract 1
- 238000000605 extraction Methods 0.000 abstract 1
- 239000012466 permeate Substances 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
- G01N15/0826—Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N15/0806—Details, e.g. sample holders, mounting samples for testing
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- Dispersion Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention relates to a device and a method for measuring permeability of PE (polyethylene) pipe material under mixed hydrogen natural gas, which mainly comprise a gas supply system, an insulating stainless steel permeation pool, a temperature controller, a refrigeration system and an air extraction system, wherein H with different concentrations 2 And CH 4 The mixed gas enters the insulating stainless steel infiltration tank through the gas supply system, then permeates through the PE pipe material, and the permeability can be calculated through a permeability calculation formula. The invention sets a pressure regulator in the gas supply system to regulate the outlet pressure of the gas, and an electrochemical sensor measures the concentration of the gas. A gas flowmeter is arranged at a gas outlet of the permeation tank to detect the flow of gas permeated out, a temperature controller and a refrigerating system are arranged around the permeation tank to change the temperature of the permeation tank and detect the influence of different temperatures on the permeability of the gas permeating the PE pipe. The invention can realize vacuum degree experiment conditions, improve the experimental precision of permeability, and is suitable for measuring the permeability of the PE pipe material under different pressures, concentrations and temperatures.
Description
Technical Field
The invention relates to a device and a method for measuring permeability of a PE (polyethylene) pipe material under hydrogen-mixed natural gas, belonging to the technical field of gas permeability test of a high-molecular film material.
Background
As a clean and renewable energy source, hydrogen is an ideal interconnection medium for promoting the clean and efficient utilization of the traditional fossil energy and supporting the large-scale development of the renewable energy. The hydrogen production by renewable energy is an effective way for solving the problem of green power consumption such as wind, light and the like in China, but the problem of high storage and transportation cost of hydrogen is a huge problem.
The hydrogen is doped into the natural gas, which is a good transition method for solving large-scale and long-distance hydrogen transportation, but the metal material is likely to generate hydrogen brittleness problem under the hydrogen environment, so that system components are failed, and even major accidents are caused. The influence of hydrogen on the polyethylene pipeline is small, the material has no degradation phenomenon in long-term service performance in a hydrogen environment, the microstructure of the material is not obviously changed, and the hydrogen and the polyethylene pipeline hardly interact. However, the hydrogen-loaded pipeline is easy to leak, and the hydrogen has lower density and molecular volume than methane and higher permeation rate than methane, so that the hydrogen-loaded natural gas pipeline is easy to leak, especially in nonmetal (such as PE and PVC) pipelines.
Therefore, the invention designs a device and a method for measuring permeability of a PE pipe material under hydrogen-mixed natural gas.
Disclosure of Invention
The invention aims to provide a device and a method for measuring permeability of a PE pipe material under a mixed hydrogen natural gas, which are designed from the viewpoint of ensuring safety of the PE pipe for conveying the mixed hydrogen natural gas and comprehensively analyzing various influence factors of permeability measurement, so that the permeability of the PE pipe material is measured under various hydrogen mixing ratios, and a reliable basis is provided for safe operation of the PE pipe for conveying the mixed hydrogen natural gas.
The invention mainly solves the following problems:
(1) An electrochemical sensor capable of detecting gas concentration is designed to detect the permeability of PE tube materials under hydrogen-mixed natural gas of different proportions.
(2) And a pressure regulator is arranged on the gas cylinder, the pressure of output gas is regulated, and the influence of different pressures on the permeability of the PE tube material under different hydrogen doping ratios is detected.
(3) The temperature regulator is arranged in the insulating stainless steel infiltration tank, so that the temperature in the infiltration tank can be increased, and the influence of high temperature on the permeability of the PE pipe material under different hydrogen-doping ratios can be detected.
(4) Set up refrigerating system at insulating stainless steel infiltration pond, can reduce the temperature in the infiltration pond, detect the influence of low temperature PE tube material permeability under to different hydrogen-doped ratio.
In order to achieve the above object, the present invention provides the following.
A PE pipe material permeability measuring device under hydrogen-mixed natural gas comprises a first pressure regulator 1, a second pressure regulator 2, a first valve 3, a second valve 4, an electrochemical sensor 5, a gas storage tank 6, a pressure gauge 7, a first vacuum gauge 8, a third valve 9, a downstream pressure sensor 10, a second vacuum gauge 11, an insulated stainless steel permeation cell 12, a permeation cell inlet safety valve 13, a permeation cell outlet safety valve 14, a temperature controller 15, a gas flow meter 16, a gas recovery bottle 17, an upstream pressure sensor 18, a first vacuum pump 19, a second vacuum pump 20, a fourth valve 21, a fifth valve 22 and a refrigerating system 23;
the first pressure regulator 1 and the second pressure regulator 2 are connected to a gas cylinder, a hydrogen cylinder connected with the pressure regulator 1 is connected with a first valve 3 through a pipeline, a methane cylinder connected with the pressure regulator 2 is connected with a second valve 4 through a pipeline, the first valve 3 and the second valve 4 are connected with an electrochemical sensor 5 through a pipeline, the electrochemical sensor 5 is connected with a gas storage tank 6 through a pipeline, the gas storage tank 6 is connected with a third valve 9 through a pipeline, a pressure gauge 7, a vacuum gauge 8 and a second vacuum pump 20 are connected around the gas storage tank 6, the third valve 9 is connected with a permeation pool inlet safety valve 13 through a pipeline, a downstream pressure sensor 10, a vacuum gauge 11, a vacuum pump 19, an upstream pressure sensor 13, a temperature controller 15 and a refrigeration system 23 are connected to the insulating stainless steel permeation pool 12, an outlet safety valve 14 of the permeation pool is connected with a gas flow meter 16 through a pipeline, and the gas flow meter 16 is connected with a gas recovery cylinder 17 through a pipeline.
Further, the electrochemical sensor 5 includes a gas diffusion barrier layer 51, an electrolyte 52, a separator 53, a current collector 54, a sensor pin 55, a counter electrode 56, a reference electrode 57, a sensing electrode 58;
further, the gas diffusion barrier layer 51 is formed by the measured gas passing through the electrode surface, the measured gas reacts with the sensing electrode 58 to form a sufficient electric signal, the reference electrode 57 is installed in the electrolyte 52, the fixed voltage value on the sensing electrode 58 is maintained, the measured gas molecules react with the sensing electrode 58, and the counter electrode 56 is measured, and the measurement result is usually directly related to the gas concentration.
The insulating stainless steel infiltration tank 12 comprises a pressure head 121, a sealing ring 122, a cylinder barrel 123, a PE film 124, a flange 125, a base 126, a stainless steel sintering disc 127 and a PE film infiltration sample supporting seat 128;
further, the pressure head 121 and the base 126 are provided with an inlet and an outlet, the bottom of the cylinder 123 is welded with a flange 125 and added with an axial O-shaped sealing ring, the PE film is clamped in the middle of a sintered stainless steel disc 127, a layer of PE film permeation sample supporting seat 128 covers the stainless steel sintered disc 127, the PE film permeation sample supporting seat 128 is made of stainless steel material, and a plurality of small ventilation circular holes are uniformly formed in the PE film permeation sample supporting seat 128.
The temperature controller 15 comprises 500K resistors 151, 0.47 mu capacitors 152, 1N4007 silicon integral diodes 153, 47 mu capacitors 154, 2CW71 silicon integral diodes 155, 1M resistors 156, 100 mu capacitors 157, ICs 158, potentiometers 159, electric heaters 160, bidirectional thyristors 161, 15K resistors 162, thermistors 163 and 200 omega resistors 164;
furthermore, the potential of the pin 2 of the IC158 is lower than 1/3 of the Ec voltage, the pin 3 of the IC158 outputs high level to trigger the bidirectional brake tube 161 to be conducted, the electric heater 160 is switched on to heat, the timing cycle is not started, when the temperature of the thermistor 163 at the temperature measuring point is higher than the set value, the timing cycle is not completed, the electric heater 160 is switched off after the timing cycle is ended, when the temperature of the thermistor 163 is reduced to be lower than the set value, the bidirectional brake tube 161 is triggered to be conducted again, the electric heater 160 is switched on to heat, and thus the purpose of temperature control can be achieved.
The refrigerating system 23 comprises a compressor 231, a suction pipe drier-filter 232, an evaporator pressure regulator 233, an evaporator 234, a pressure stabilizer 235, a thermostatic expansion valve 236, a liquid moisture indicator 237, a solenoid valve 238, a drier-filter 239, an accumulator 240, a pressure difference controller 241, a condenser 242, and a muffler 243;
further, the compressor 231, the air intake pipe filter drier 232, the evaporator pressure regulator 233, the evaporator 234 pressure stabilizer 235, the thermostatic expansion valve 236, the liquid moisture indicator 237, the solenoid valve 238, the filter drier 239, the accumulator 240, the pressure difference controller 241, the condenser 242, and the muffler 243 are sequentially connected by a conduit, the compressor 231 sucks low-temperature and low-pressure refrigerant vapor from the evaporator, adiabatically compresses the refrigerant vapor into high-temperature and high-pressure superheated vapor by the compressor 231, then presses the superheated vapor into the condenser 242 for constant-pressure cooling, and releases heat to the cooling medium, and then cools the refrigerant into a supercooled liquid refrigerant, the liquid refrigerant adiabatically throttles the refrigerant into a low-pressure liquid refrigerant by the thermostatic expansion valve 236, and evaporates and absorbs heat in air in the evaporator 234, thereby cooling the air to achieve the purpose of cooling.
A method for measuring permeability of PE tube material under mixed hydrogen natural gas comprises the following steps:
a. before the test, a PE pipe material sample is arranged in an insulating stainless steel infiltration tank 12, wherein the PE pipe material sample adopts a circular film with the thickness of 0.3mm-1 mm;
b. after the PE pipe material sample is installed, starting a vacuum pump 19 and a vacuum pump 20 to pump the insulating stainless steel permeation cell 12 and the gas storage tank 6 to reach a vacuum condition;
c. enabling the hydrogen to reach a pressure value required by a test through the first pressure regulator 1, then opening the first valve 3, detecting the concentration of the hydrogen through the electrochemical sensor 5, and closing the first valve 3 when the concentration of the hydrogen reaches a concentration value required by the test;
d. the second pressure regulator 2 is used for enabling methane to reach a pressure value required by a test, then the second valve 4 is opened, the concentration of the methane is detected by the electrochemical sensor 5, when the concentration of the hydrogen reaches a concentration value required by the test, the second valve 4 is closed, and a mixture of the hydrogen and the methane with the concentration required by the test is stored in the gas storage tank 6;
e. the temperature in the insulating stainless steel infiltration tank 12 is adjusted to the temperature required by the test through the adjustment of a temperature controller 15;
f. opening the third valve 9, introducing the hydrogen and methane mixed gas into the insulating stainless steel permeation pool 12, and measuring the flow Q of the permeated gas by the gas flowmeter 16 0 Downflow pressure sensor 10 for measuring PE pipe samplePressure P downstream of the product 1 Upstream pressure sensor 18 measures the pressure P upstream of the PE tube material sample 2 The permeated gas mixture finally flows into the gas recovery bottle 17;
g. permeability calculated by formula
h. Wherein k is g Is gas permeability μm 2 (ii) a A is the sectional area cm of a PE pipe material sample 2 (ii) a L is the diameter cm and Q of the PE pipe 0 Is the gas flow cm 3/ s；p 0 Is at atmospheric pressure; mu.s g Is gas viscosity mpa.s; p is a radical of 1 、p 2 Downstream and upstream pressures Mpa for PE tube material, respectively.
i. Repeating the steps a to d, and adjusting the temperature in the insulating stainless steel infiltration tank 12 to the temperature required by the test through a refrigeration system 23;
j. repeating c-g;
k. the pressure value adjusting range in the steps c and d is 0.1MPa-10MPa, the concentration of hydrogen is (0%, 10%, 20%, 50%, 100%), the concentration of methane is (100%, 90%, 80%, 50%, 0%), the temperature adjusting range in the step e is (15 ℃ -100 ℃), and the temperature adjusting range in the step h is (-40 ℃ -0 ℃).
Drawings
Fig. 1 is a schematic structural diagram of a device for measuring permeability of a PE tube material under hydrogen-mixed natural gas in the practice of the present invention.
FIG. 2 is a schematic diagram of the structure of an electrochemical sensor in the practice of the present invention.
Fig. 3 is a schematic diagram of the structure of an insulated stainless steel infiltration tank in the practice of the present invention.
FIG. 4 is a schematic circuit diagram of a temperature controller in an embodiment of the present invention.
Figure 5 is a schematic diagram of a refrigeration system in the practice of the present invention.
Detailed Description
The following description of specific embodiments of the present invention is provided in order to better understand the present invention with reference to the accompanying drawings.
Examples
In this embodiment, fig. 1 shows that the permeability measuring device of the PE tube material under the hydrogen-mixed natural gas includes a first pressure regulator 1, a second pressure regulator 2, a first valve 3, a second valve 4, an electrochemical sensor 5, a gas storage tank 6, a pressure gauge 7, a first vacuum gauge 8, a third valve 9, a downstream pressure sensor 10, a second vacuum gauge 11, an insulating stainless steel permeation cell 12, a permeation cell inlet safety valve 13, a permeation cell outlet safety valve 14, a temperature controller 15, a gas flowmeter 16, a gas recovery bottle 17, an upstream pressure sensor 18, a first vacuum pump 19, a second vacuum pump 20, a fourth valve 21, a fifth valve 22, and a refrigeration system 23;
the first pressure regulator 1 and the second pressure regulator 2 are connected to a gas cylinder, a hydrogen cylinder connected with the pressure regulator 1 is connected with a first valve 3 through a pipeline, a methane cylinder connected with the pressure regulator 2 is connected with a second valve 4 through a pipeline, the first valve 3 and the second valve 4 are connected with an electrochemical sensor 5 through a pipeline, the electrochemical sensor 5 is connected with a gas storage tank 6 through a pipeline, the gas storage tank 6 is connected with a third valve 9 through a pipeline, a pressure gauge 7, a vacuum gauge 8 and a second vacuum pump 20 are connected around the gas storage tank 6, the third valve 9 is connected with a permeation pool inlet safety valve 13 through a pipeline, a downstream pressure sensor 10, a vacuum gauge 11, a vacuum pump 19, an upstream pressure sensor 13, a temperature controller 15 and a refrigeration system 23 are connected to the insulating stainless steel permeation pool 12, an outlet safety valve 14 of the permeation pool is connected with a gas flow meter 16 through a pipeline, and the gas flow meter 16 is connected with a gas recovery cylinder 17 through a pipeline.
Fig. 2 is a schematic diagram of the structure of an electrochemical sensor 5 according to the present invention, wherein the electrochemical sensor comprises a gas diffusion barrier layer 51, an electrolyte 52, a separator 53, a current collector 54, a sensor pin 55, a counter electrode 56, a reference electrode 57, and a sensing electrode 58;
the gas diffusion barrier layer 51 is formed by the measured gas passing through it to the electrode surface, the measured gas reacts with the sensing electrode 58 to form a sufficient electrical signal, the reference electrode 57 is installed in the electrolyte 52, the fixed voltage value on the sensing electrode 58 is maintained, the measured gas molecules react with the sensing electrode 58, and the counter electrode 56 is measured, the measurement result is usually directly related to the gas concentration.
Fig. 3 is a schematic structural diagram of an insulating stainless steel infiltration tank in the practice of the present invention, wherein the insulating stainless steel infiltration tank 12 comprises a pressure head 121, a sealing ring 122, a cylinder 123, a PE film 124, a flange 125, a base 126, a stainless steel sintered disc 127 and a PE film infiltration sample supporting seat 128;
the pressure head 121 and the base 126 are provided with an air inlet and an air outlet, the bottom of the cylinder 123 is welded with a flange 125 and is added with an axial O-shaped sealing ring, the PE film is clamped in the middle of a sintered stainless steel disc 127, a layer of PE film permeation sample supporting seat 128 covers the stainless steel sintered disc 127, and the PE film permeation sample supporting seat 128 is made of stainless steel materials and is uniformly provided with a plurality of air vents.
FIG. 4 is a schematic circuit diagram of a temperature controller in the practice of the present invention, in which the components of the temperature controller 15 include a 500K resistor 151, a 0.47 μ capacitor 152, a 1N4007 silicon diode 153, a 47 μ capacitor 154, a 2CW71 silicon diode 155, a 1M resistor 156, a 100 μ capacitor 157, an IC158, a potentiometer 159, an electric heater 160, a bidirectional thyristor 161, a 15K resistor 162, a thermistor 163, and a 200 Ω resistor 164;
the potential of the pin 2 of the IC158 is lower than 1/3 of the Ec voltage, the pin 3 of the IC158 outputs high level to trigger the bidirectional brake tube 161 to conduct, the electric heater 160 is switched on to heat, the timing cycle is not started, when the temperature of the thermistor 163 at the temperature measuring point is higher than the set value, the timing cycle is not completed, the electric heater 160 is switched off after the timing cycle is ended, when the temperature of the thermistor 163 is reduced to be lower than the set value, the bidirectional brake tube 161 is triggered to conduct again, the electric heater 160 is switched on to heat, and thus the purpose of temperature control can be achieved.
Fig. 5 is a schematic diagram of a refrigeration system in which the compressor 231, the suction pipe filter drier 232, the evaporator pressure regulator 233, the evaporator 234, the pressure stabilizer 235, the thermostatic expansion valve 236, the liquid moisture indicator 237, the solenoid valve 238, the filter drier 239, the accumulator 240, the differential pressure controller 241, the condenser 242, and the muffler 243 of the refrigeration system 23 are shown;
the compressor 231 sucks low-temperature and low-pressure refrigerant steam from the evaporator, the low-temperature and low-pressure refrigerant steam is adiabatically compressed into high-temperature and high-pressure superheated steam by the compressor 231, the high-temperature and high-pressure superheated steam is then pressed into the condenser 242 for constant pressure cooling and releases heat to a cooling medium, and then the high-temperature and high-pressure superheated steam is cooled into a sub-cooling liquid refrigerant, the liquid refrigerant is adiabatically throttled by the thermostatic expansion valve 236 to become a low-pressure liquid refrigerant, and the heat in the air is evaporated and absorbed in the evaporator 234, so that the purpose of cooling the air is achieved.
A method for measuring permeability of PE tube material under mixed hydrogen natural gas comprises the following steps:
a. before the test is started, a PE tube material sample is arranged in an insulating stainless steel infiltration tank 12, and a circular film with the thickness of 0.3mm-1mm is adopted as the PE tube material sample;
b. after the PE pipe material sample is installed, starting a vacuum pump 19 and a vacuum pump 20 to pump the insulating stainless steel permeation cell 12 and the gas storage tank 6 to reach a vacuum condition;
c. enabling the hydrogen to reach a pressure value required by a test through the first pressure regulator 1, then opening the first valve 3, detecting the concentration of the hydrogen through the electrochemical sensor 5, and closing the first valve 3 when the concentration of the hydrogen reaches a concentration value required by the test;
d. the second pressure regulator 2 is used for enabling methane to reach a pressure value required by a test, then the second valve 4 is opened, the concentration of the methane is detected by the electrochemical sensor 5, when the concentration of the hydrogen reaches a concentration value required by the test, the second valve 4 is closed, and a mixture of the hydrogen and the methane with the concentration required by the test is stored in the gas storage tank 6;
e. the temperature in the insulating stainless steel infiltration tank 12 is adjusted to the temperature required by the test through the adjustment of a temperature controller 15;
f. opening the third valveThe door 9, the mixed gas of hydrogen and methane enters an insulating stainless steel permeation pool 12, and the flow Q of the permeated gas is measured by a gas flowmeter 16 0 Downstream pressure sensor 10 measures pressure P downstream of the PE tube material sample 1 Upstream pressure sensor 18 measures the pressure P upstream of the PE tube material sample 2 The permeated gas mixture finally flows into the gas recovery bottle 17;
g. permeability calculated by formula
h. Wherein k is g Is gas permeability μm 2 (ii) a A is the sectional area cm of a PE pipe material sample 2 (ii) a L is the diameter cm and Q of the PE pipe 0 Is the gas flow rate cm 3/ s；p 0 Is at atmospheric pressure; mu.s g Is a gas viscosity mpa.s; p is a radical of formula 1 、p 2 Downstream and upstream pressures Mpa for PE tube material, respectively. i. Repeating the steps a to d, and adjusting the temperature in the insulating stainless steel infiltration tank 12 to the temperature required by the test through a refrigeration system 23;
j. repeating c-g;
k. the pressure value adjusting range in the steps c and d is 0.1MPa-10MPa, the concentration of hydrogen is (0%, 10%, 20%, 50%, 100%), the concentration of methane is (100%, 90%, 80%, 50%, 0%), the temperature adjusting range in the step e is (15 ℃ -100 ℃), and the temperature adjusting range in the step h is (-40 ℃ -0 ℃).
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (6)
1. A PE pipe material permeability measuring device and method under hydrogen-mixed natural gas are characterized in that: the device comprises a first pressure regulator (1), a second pressure regulator (2), a first valve (3), a second valve (4), an electrochemical sensor (5), a gas storage tank (6), a pressure gauge (7), a first vacuum gauge (8), a third valve (9), a downstream pressure sensor (10), a second vacuum gauge (11), an insulated stainless steel infiltration tank (12), an infiltration tank inlet safety valve (13), an infiltration tank outlet safety valve (14), a temperature controller (15), a gas flowmeter (16), a gas recovery bottle (17), an upstream pressure sensor (18), a first vacuum pump (19), a second vacuum pump (20), a fourth valve (21), a fifth valve (22) and a refrigeration system (23);
the gas recovery system comprises a first pressure regulator (1), a second pressure regulator (2), a hydrogen cylinder connected with the pressure regulator (1) and connected with a first valve (3) through a pipeline, a methane cylinder connected with the pressure regulator (2) and connected with a second valve (4) through a pipeline, the first valve (3) and the second valve (4) are connected with an electrochemical sensor (5) through a pipeline, the electrochemical sensor (5) is connected with a gas storage tank (6) through a pipeline, the gas storage tank (6) is connected with a third valve (9) through a pipeline, a pressure gauge (7), a vacuum gauge (8) and a second vacuum pump (20) are connected around the gas storage tank (6), the third valve (9) is connected with a permeation pool inlet safety valve (13) through a pipeline, a downstream pressure sensor, a vacuum gauge (11), a vacuum pump (19), an upstream pressure sensor (13) and a temperature controller (15) and a refrigeration system (23) are connected with an insulating stainless steel permeation pool (12) through a pipeline, a downstream pressure sensor, a vacuum gauge (11), a vacuum gauge (13), an upstream pressure sensor (13) and a gas flowmeter (16) are connected with a gas recovery cylinder (17).
2. The apparatus for measuring permeability of PE tube material under mixed hydrogen natural gas according to claim 1, wherein: the electrochemical sensor (5) comprises a gas diffusion barrier layer (51), an electrolyte (52), a separator (53), a current collector (54), a sensor pin (55), a counter electrode (56), a reference electrode (57), and a sensing electrode (58);
the gas diffusion barrier layer (51) is used for allowing the measured gas to pass through and reach the surface of the electrode, the measured gas reacts with the sensing electrode (58) to form a sufficient electric signal, the reference electrode (57) is arranged in the electrolyte (52) and maintains the fixed voltage value on the sensing electrode (58), the measured gas molecules react with the sensing electrode (58), and meanwhile, the counter electrode (56) is measured, and the measurement result is generally directly related to the gas concentration.
3. The apparatus for measuring permeability of PE tube material under mixed hydrogen natural gas according to claim 1, wherein: the insulating stainless steel infiltration tank (12) comprises a pressure head (121), a sealing ring (122), a cylinder barrel (123), a PE film (124), a flange (125), a base (126), a stainless steel sintered disc (127) and a PE film infiltration sample supporting seat (128);
the pressure head (121) and the base (126) are provided with an inlet and an outlet, a flange (125) is welded at the bottom of the cylinder barrel (123) and an axial O-shaped sealing ring is added, the PE film is clamped in the middle of a sintered stainless steel disc (127), a layer of PE film permeation sample supporting seat (128) covers the stainless steel sintered disc (127), and the PE film permeation sample supporting seat (128) is made of stainless steel materials and is uniformly provided with a plurality of vent holes.
4. The device for measuring permeability of PE tube material under mixed hydrogen natural gas according to claim 1, wherein: the temperature controller (15) comprises components including a 500K resistor (151), a 0.47 mu capacitor (152), a 1N4007 silicon integral diode (153), a 47 mu capacitor (154), a 2CW71 silicon integral diode (155), a 1M resistor (156), a 100 mu capacitor (157), an IC (158), a potentiometer (159), an electric heater (160), a bidirectional thyristor (161), a 15K resistor (162), a thermistor (163) and a 200 omega resistor (164);
the potential of 2 pins of the IC (158) is lower than 1/3 of Ec voltage, 3 pins of the IC (158) output high level to trigger the bidirectional brake tube (161) to be conducted, the electric heater (160) is switched on to heat, a timing cycle is never started, when the temperature of the thermistor (163) arranged at a temperature measuring point is higher than a set value, and the timing cycle is not completed, the electric heater (160) is switched off after a timing period is ended, when the temperature of the thermistor (163) is reduced to be lower than the set value, the bidirectional brake tube (161) is triggered to be conducted again, the electric heater (160) is switched on to heat, and thus the purpose of temperature control can be achieved.
5. The device for measuring permeability of PE tube material under mixed hydrogen natural gas according to claim 1, wherein: the refrigeration system (23) is characterized in that the compressor (231), the air suction pipe drying filter (232), the evaporator pressure regulator (233), the evaporator (234), the pressure stabilizer (235), the thermostatic expansion valve (236), the liquid moisture indicator (237), the electromagnetic valve (238), the drying filter (239), the accumulator (240), the pressure difference controller (241), the condenser (242) and the silencer (243) are sequentially connected through a conduit;
the compressor (231) sucks low-temperature and low-pressure refrigerant steam from the evaporator, the refrigerant steam is adiabatically compressed into high-temperature and high-pressure superheated steam through the compressor (231), the superheated steam is then pressed into the condenser (242) for constant-pressure cooling and releases heat to a cooling medium, then the refrigerant is cooled into a supercooled liquid refrigerant, the liquid refrigerant is adiabatically throttled by the thermostatic expansion valve (236) to become low-pressure liquid refrigerant, and the low-pressure liquid refrigerant is evaporated in the evaporator (234) to absorb heat in air, so that the air is cooled to achieve the purpose of refrigeration.
6. A method for measuring permeability of PE tube material under hydrogen-mixed natural gas is characterized in that: the method comprises the following steps:
a. before the test is started, a PE pipe material sample is arranged in an insulating stainless steel infiltration tank (12), and a circular thin film with the thickness of 0.3mm-1mm is adopted by the PE pipe material sample;
b. after the PE pipe material sample is installed, starting a vacuum pump (19) and a vacuum pump (20) to pump air in an insulating stainless steel permeation pool (12) and an air storage tank (6) to achieve a vacuum condition;
c. enabling the hydrogen to reach a pressure value required by a test through a first pressure regulator (1), then opening a first valve (3), detecting the concentration of the hydrogen through an electrochemical sensor (5), and closing the first valve (3) when the concentration of the hydrogen reaches a concentration value required by the test;
d. the methane reaches the pressure value required by the test through the second pressure regulator (2), then the second valve (4) is opened, the concentration of the methane is detected by the electrochemical sensor (5), when the concentration of the hydrogen reaches the concentration value required by the test, the second valve (4) is closed, and the mixture of the hydrogen and the methane with the concentration required by the test is stored in the gas storage tank (6);
e. the temperature in the insulating stainless steel infiltration tank (12) is adjusted to the temperature required by the test through the adjustment of a temperature controller (15);
f. opening the third valve (9), introducing the hydrogen and methane mixed gas into an insulating stainless steel permeation pool (12), and measuring the flow Q of the permeated gas by a gas flow meter (16) 0 A downstream pressure sensor (10) measures the pressure P downstream of the PE tube material sample 1 An upstream pressure sensor (18) measures the pressure P upstream of the PE tube material sample 2 The permeated gas mixture finally flows into a gas recovery bottle (17);
g. permeability calculated by formula
Wherein k is g Is gas permeability μm 2 (ii) a A is the sectional area cm of a PE pipe material sample 2 (ii) a L is the diameter cm and Q of the PE pipe 0 Is the gas flow cm 3/ s；p 0 Is at atmospheric pressure; mu.s g Is a gas viscosity mpa.s; p is a radical of 1 、p 2 Downstream pressure and upstream pressure Mpa of PE pipe material respectively;
h. repeating the steps a to d, and adjusting the temperature in the insulating stainless steel infiltration tank (12) to the temperature required by the test through a refrigeration system (23);
i. repeating c-g;
j. the pressure value adjusting range in the steps c and d is 0.1MPa-10MPa, the concentration of hydrogen is (0%, 10%, 20%, 50%, 100%), the concentration of methane is (100%, 90%, 80%, 50%, 0%), the temperature adjusting range in the step e is (15 ℃ -100 ℃), and the temperature adjusting range in the step h is (-40 ℃ -0 ℃).
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