CN114486079A - Air tightness detection method of diaphragm - Google Patents
Air tightness detection method of diaphragm Download PDFInfo
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- CN114486079A CN114486079A CN202111585856.6A CN202111585856A CN114486079A CN 114486079 A CN114486079 A CN 114486079A CN 202111585856 A CN202111585856 A CN 202111585856A CN 114486079 A CN114486079 A CN 114486079A
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- 238000001514 detection method Methods 0.000 title claims description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 280
- 239000001257 hydrogen Substances 0.000 claims abstract description 274
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 274
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 215
- 239000001301 oxygen Substances 0.000 claims abstract description 215
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 215
- 239000007789 gas Substances 0.000 claims abstract description 93
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 47
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 42
- 239000003792 electrolyte Substances 0.000 claims abstract description 36
- 238000012360 testing method Methods 0.000 claims abstract description 29
- 238000010835 comparative analysis Methods 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 12
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 9
- 229910001882 dioxygen Inorganic materials 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000009434 installation Methods 0.000 claims description 6
- 230000001276 controlling effect Effects 0.000 claims description 5
- 210000001503 joint Anatomy 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000010425 asbestos Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/005—H2
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Abstract
The invention discloses a method for detecting the air tightness of a diaphragm, which comprises the steps of installing the first step, adding electrolyte in the second step, introducing gas in the third step, performing a boost test in the fourth step, performing a parallel test in the fifth step and performing comparative analysis in the sixth step, wherein the method for detecting the air tightness of the diaphragm simulates the working condition of the diaphragm in a water electrolysis hydrogen production device, can detect the applicable pressure range of the diaphragm to be detected, and can judge the advantages and disadvantages of the air tightness of the diaphragm to be detected and the diaphragm used for comparison through the parallel experiment, so that whether the diaphragm to be detected can be used in the water electrolysis hydrogen production device with rated pressure or variable pressure can be judged, and the purity of hydrogen and oxygen produced by the water electrolysis hydrogen production device can be further improved.
Description
Technical Field
The invention belongs to the technical field of membrane air tightness detection, and particularly relates to an air tightness detection method for a membrane in a water electrolysis hydrogen production device.
Background
Membranes are commonly used in hydrogen production plants or filtration plants. The material of the diaphragm used in the water electrolysis hydrogen production device is usually asbestos cloth, and the air tightness of the diaphragm made of the material is measured by an air tightness measuring device in the asbestos cloth of the diaphragm of the building material industry standard JC/T211-2009 of the people's republic of China at present. The device includes: the upper end and the lower end of the lower cylinder are provided with openings, the bottom end of the lower cylinder is provided with a bottom flange, the top end of the lower cylinder is provided with an opening, a top flange and a lower cylinder with a closed bottom end, the side wall of the lower end of the lower cylinder is provided with a water inlet pipe and a water outlet pipe, the water inlet pipe is provided with a water inlet valve, the water outlet pipe is provided with a water outlet valve, and the side wall of the upper end of the lower cylinder is provided with a U-shaped pressure indicating pipe. When the air tightness of a newly developed diaphragm needs to be detected, the specific detection method comprises the following steps: firstly, installation: clamping a diaphragm to be detected between a bottom flange of the upper cylinder and a top flange of the lower cylinder, wherein the upper cylinder and the lower cylinder are in sealed butt joint through the bottom flange and the top flange, and the diaphragm separates inner cavities of the upper cylinder and the lower cylinder; secondly, detection: closing the water inlet valve and the water outlet valve, adding quantitative water into an upper space formed by the diaphragm to be detected and the upper cylinder, opening the water inlet valve, enabling the water to enter a lower space formed by the lower cylinder and the diaphragm to be detected, gradually reducing the volume of gas in the lower space, gradually increasing the pressure in the lower space, enabling a liquid level difference to appear in the U-shaped pressure indicating pipe, and recording the liquid level difference in the U-shaped pressure indicating pipe to be H1 when a first bubble appears in the water in the upper space; thirdly, performing a parallel experiment: and (3) clamping a diaphragm with known air tightness between a bottom flange of the upper cylinder and a top flange of the lower cylinder, repeating the detection step, recording the liquid level difference in the U-shaped pressure indicating pipe at the moment as H2 when a first air bubble appears in the water in the upper space, judging that the air tightness of the diaphragm to be detected is better than that of the diaphragm with known air tightness when H1 is larger than H2, and conversely, judging that the air tightness of the diaphragm to be detected is worse than that of the diaphragm with known air tightness when H1 is smaller than H2.
At present, the hydrogen production apparatus by water electrolysis commonly used in industry comprises: the hydrogen production electrolytic tank is connected with a power supply at two ends, and is internally provided with: the hydrogen production electrolytic cell is divided into a diaphragm of an anode region and a cathode region, an electrode anode is arranged in the anode region, an electrode cathode is arranged in the cathode region, and when the hydrogen production electrolytic cell works, electrolyte is filled in the cell, wherein the electrolyte is usually potassium hydroxide solution or sodium hydroxide solution. After the power supply is switched on, oxygen is generated in the anode region, hydrogen is generated in the cathode region, and in the working process of the water electrolysis hydrogen production device, the diaphragm in the hydrogen production electrolytic cell needs to meet the air tightness requirement of the water electrolysis hydrogen production device, so that the danger caused by mutual connection of the hydrogen in the cathode region and the oxygen in the anode region is prevented.
When the water electrolysis hydrogen production device works, water in the electrolyte is electrolyzed into oxygen and hydrogen, the yield of the hydrogen is 2 times of that of the oxygen, and the diaphragm is vertically arranged and is always immersed in the electrolyte in the hydrogen production electrolytic cell. According to different power supplies adopted by the water electrolysis hydrogen production device, the pressure in the hydrogen production device has rated pressure and variable pressure. If the water electrolysis hydrogen production device adopts a power supply with stable voltage, the pressure in the hydrogen production device has two rated pressures of 1.6MPa and 3.2 MPa; if the power supply is provided by renewable energy sources such as wind energy and solar energy, the electric energy generated by the renewable energy sources is changed all the time, and the electric power in the hydrogen production device needs to be adjustable at high frequency, the pressure in the water electrolysis hydrogen production device is changed within the pressure range of 0.1-3.2 MPa; and when the water electrolysis hydrogen production device works, the pressure difference between the cathode region and the anode region at the two sides of the diaphragm is not more than 0.1 kPa.
As can be seen from the above, the operating conditions of the separator in the hydrogen production by water electrolysis apparatus and the operating conditions of the airtightness measuring apparatus in JC/T211-2009 standard are different: the pressure range of the water electrolysis hydrogen production device is 0.1-3.2 MPa, the pressure difference between a cathode region and an anode region on two sides of a diaphragm is not more than 0.1kPa, when the air tightness measuring device in JC/T211-2009 standard works, the pressure in an upper space is normal pressure, the pressure in a lower space is greater than the pressure in the upper space, and the pressure difference on two sides of the diaphragm is greater. And secondly, a diaphragm in the industrial water electrolysis hydrogen production device is vertically arranged and is always immersed in the electrolyte, and the diaphragm in the air tightness measuring device in the JC/T211-2009 standard is horizontally arranged, and the upper surface of the diaphragm is in contact with water, and the lower surface of the diaphragm is in contact with air. It can be seen that, because the detected working condition of the separator gas tightness measuring device is greatly different from the working condition of the separator in actual use, the gas tightness performance of the separator in the gas tightness measuring device is also greatly different from the gas tightness performance of the separator in the water electrolysis hydrogen production device, and a large error exists when the gas tightness result of the separator to be detected, which is determined by the gas tightness measuring device and the detecting method thereof in the JC/T211-2009 standard, is used for judging whether the separator can be used in the water electrolysis hydrogen production device.
Disclosure of Invention
The purpose of the invention is: the air tightness detection method can simulate the working conditions of the diaphragm in the water electrolysis hydrogen production device, detect the diaphragm to be detected by adopting the air tightness detection method, detect the applicable safe working pressure range of the diaphragm to be detected, and judge whether the diaphragm to be detected can be used in the water electrolysis hydrogen production device with rated pressure or variable pressure.
In order to achieve the purpose, the invention adopts the technical scheme that: the air tightness detection method of the diaphragm comprises the following steps:
the method comprises the following steps: installation: installing a diaphragm for comparison in a water electrolysis hydrogen production device with rated pressure of 1.6MPa and 3.2MPa in a closed container, vertically arranging the diaphragm for comparison, dividing the inner cavity of the container into an oxygen side space and a hydrogen side space, opening an oxygen side stop valve on an oxygen side discharge pipe communicated with the oxygen side space, wherein the oxygen side space can be communicated with the outside, opening a hydrogen side stop valve on a hydrogen side discharge pipe communicated with the hydrogen side space, and the hydrogen side space can be communicated with the outside;
step two: adding an electrolyte: adding electrolyte into the inner cavity of the container until the electrolyte submerges the diaphragm for comparison;
step three: introducing gas: oxygen enters electrolyte in the oxygen side space through an oxygen side gas inlet pipe communicated with the oxygen side space, hydrogen enters electrolyte in the hydrogen side space through a hydrogen side gas inlet pipe communicated with the hydrogen side space, and the flow of the hydrogen entering the hydrogen side space is controlled to be 2 times of the flow of the oxygen entering the oxygen side space; in the step, the pressure in the hydrogen side space is controlled to be more than the normal pressure and less than 0.2MPa, the pressure in the oxygen side space is not less than the pressure in the hydrogen side space, and the pressure difference between the two sides is less than 0.1 kPa;
step four: and (3) boosting test: controlling the opening degree of an oxygen side stop valve and a hydrogen side stop valve to enable the pressure in an oxygen side space and a hydrogen side space to gradually rise, keeping the pressure in the oxygen side space not less than the pressure in the hydrogen side space and the pressure difference between the two sides less than 0.1kPa in the pressure rising process, after the pressure in the hydrogen side space reaches 0.2MPa, stably operating for 5-15 min in the state, detecting the content of hydrogen in gas in an oxygen side discharge pipe and the content of oxygen in gas in a hydrogen side discharge pipe in the state, recording data, then controlling the pressure to continuously rise, and detecting the content of hydrogen in gas in the oxygen side discharge pipe and the content of oxygen in gas in the hydrogen side discharge pipe in the state after the pressure in the hydrogen side space rises to a set pressure value every time, stably operating for 5-15 min in the state, and recording data respectively according to sequence until the pressure in the hydrogen side space reaches 3.2MPa, After the stable operation is carried out for 5-15 min under the state, detecting the content of hydrogen in the gas in the oxygen side discharge pipe and the content of oxygen in the gas in the hydrogen side discharge pipe under the state and respectively recording the contents; thus, through the operation process, the content data of the hydrogen in the gas in the oxygen side discharge pipe can form an oxygen side comparison data set, and the content data of the oxygen in the gas in the hydrogen side discharge pipe can form a hydrogen side comparison data set;
step five: and (3) parallel testing: dismantling the diaphragms used for comparison in the container, installing the diaphragms to be detected in the container, vertically arranging the diaphragms to be detected, repeating the steps of adding electrolyte and three-way gas in the second step, and then performing the step-up test in the fourth step, wherein the difference lies in that: in the boost test step, two situations can occur: the first one is: in the process of gradually increasing the pressure, when the pressure is increased to a certain pressure value, if the content of hydrogen in the gas in the oxygen side discharge pipe is measured to exceed a set value or the content of oxygen in the gas in the hydrogen side discharge pipe is measured to exceed the set value, recording the pressure value at the moment, and ending the test, wherein the condition shows that the diaphragm to be detected can only be used in a safe working pressure range which is less than the pressure value; the second method is as follows: in the process of gradually increasing the pressure, the measured content of hydrogen in the gas in the oxygen side discharge pipe or the measured content of oxygen in the gas in the hydrogen side discharge pipe does not exceed a set value, the content of hydrogen in the gas in the oxygen side discharge pipe and the content of oxygen in the gas in the hydrogen side discharge pipe are detected and respectively recorded after the pressure in the hydrogen side space reaches 3.2MPa and the state is maintained for 5-15 min, and the test is finished, wherein the condition shows that the diaphragm to be detected can be used within the pressure range of 0.1-3.2 MPa; thus, through the parallel test process, the content data of the hydrogen in the gas in the oxygen side discharge pipe can form an oxygen side data group to be tested, and the content data of the oxygen in the gas in the hydrogen side discharge pipe can form a hydrogen side data group to be tested;
step six: and (3) comparative analysis: the specific method comprises the following steps: if the second condition occurs in the step-up test step of the diaphragm to be detected, when each data in the oxygen side to-be-detected data group is smaller than the corresponding data in the oxygen side comparison data group and each data in the hydrogen side to-be-detected data group is smaller than the corresponding data in the hydrogen side comparison data group, the fact that the air tightness of the diaphragm to be detected in the pressure range of 0.2-3.2 MPa is better than that of the diaphragm used for comparison shows that the diaphragm to be detected in the pressure range of 0.2-3.2 MPa can be used in a water electrolysis hydrogen production device with two rated pressures of 1.6MPa and 3.2MPa and can also be used in a water electrolysis hydrogen production device with variable pressure; when each datum in the front section of the oxygen side to-be-detected data set is smaller than a corresponding datum in the front section of the oxygen side comparison data set, each datum in the rear section of the oxygen side to-be-detected data set is larger than a corresponding datum in the rear section of the oxygen side comparison data set, and each datum in the front section of the hydrogen side to-be-detected data set is smaller than a corresponding datum in the front section of the hydrogen side comparison data set, and each datum in the rear section of the hydrogen side to-be-detected data set is larger than a corresponding datum in the rear section of the oxygen side comparison data set, the airtightness of the diaphragm to be detected in the front section pressure range corresponding to the front section datum is better than the airtightness of the diaphragm for comparison, and the diaphragm to be detected can be used in the water electrolysis hydrogen production device with rated pressure in the front section pressure range; if the first condition occurs in the step of the pressure-increasing test of the diaphragm to be detected, the detected oxygen side data group to be detected and the detected hydrogen side data group to be detected within the safe working pressure range of the diaphragm to be detected are compared with the corresponding data of the comparison diaphragm within the safe working pressure range one by one, and the comparison and analysis method is the same as that of the second condition.
Further, the method for detecting the airtightness of the separator includes: in the fourth step, the set pressure value is 0.1 MPa.
Further, the method for detecting the airtightness of the separator includes: in the fifth step, the set value of the hydrogen gas content in the gas in the oxygen-side discharge pipe and the set value of the oxygen gas content in the gas in the hydrogen-side discharge pipe are both 2%.
Further, the method for detecting the airtightness of the separator includes: the oxygen side discharge pipe at the front end of the oxygen side stop valve is communicated with an oxygen side detection pipe, the oxygen side detection pipe is provided with an oxygen detection valve and a hydrogen content analyzer, the hydrogen side discharge pipe at the front end of the hydrogen side stop valve is communicated with a hydrogen side detection pipe, the hydrogen side detection pipe is provided with a hydrogen detection valve and an oxygen content analyzer, the container is also provided with an oxygen side pressure transmitter for detecting the pressure in the oxygen side space and a hydrogen side pressure transmitter for detecting the pressure in the hydrogen side space, the oxygen side stop valve and the hydrogen side stop valve are electric regulating valves, the oxygen side pressure transmitter, the hydrogen side pressure transmitter, the oxygen side stop valve, the hydrogen content analyzer and the oxygen content analyzer are all in electric signal connection with the controller.
Further, the method for detecting the airtightness of the separator includes: and D, soaking the diaphragm used for comparison in the step one and the diaphragm to be detected in the step five in the electrolyte for 24 hours, and then installing.
Further, the method for detecting the airtightness of the separator includes: the container comprises an oxygen side container and a hydrogen side container, wherein the oxygen side container and the hydrogen side container are both pipes with one ends closed and the other ends opened; when the oxygen side container is installed, the membrane is vertically arranged and is clamped between the opening of the oxygen side container and the opening of the hydrogen side container, the opening of the oxygen side container is in sealed butt joint with the opening of the hydrogen side container, and the membrane separates the inner cavity of the oxygen side container from the inner cavity of the hydrogen side container.
Further, the method for detecting the airtightness of the separator includes: the oxygen side container and the hydrogen side container are both horizontally placed.
Further, the method for detecting the airtightness of the separator includes: the outlet end of the oxygen side gas inlet pipe extends into the bottom of the oxygen side space, and the outlet end of the hydrogen side gas inlet pipe extends into the bottom of the hydrogen side space.
Further, the method for detecting the airtightness of the separator includes: and after the second step is finished, replacing the air in the container and each pipeline by nitrogen, and after the nitrogen replacement is finished, performing the operation of the third step.
The invention has the advantages that: the air tightness detection method of the diaphragm simulates the working condition of the diaphragm in the water electrolysis hydrogen production device, can detect the pressure range applicable to the diaphragm to be detected, and can judge the quality of the air tightness of the diaphragm to be detected and the air tightness of the diaphragm used for comparison through parallel experiments, so that whether the diaphragm to be detected can be used in the water electrolysis hydrogen production device with rated pressure or variable pressure can be judged, and the purity of the hydrogen and oxygen produced by the water electrolysis hydrogen production device is further improved.
Drawings
Fig. 1 is a schematic view of the structural principle of a container suitable for the method for detecting the airtightness of a membrane according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to preferred embodiments.
The air tightness detection method of the diaphragm comprises the following steps:
the method comprises the following steps: installation: the diaphragm used for comparison, which is well soaked in electrolyte and known to be used in a water electrolysis hydrogen production device with rated pressure of 1.6MPa and 3.2MPa, is arranged in a container with the periphery closed, the diaphragm used for comparison is vertically arranged and divides the inner cavity of the container into an oxygen side space 1 and a hydrogen side space 2, an oxygen side stop valve 31 on an oxygen side discharge pipe 3 communicated with the oxygen side space 1 is opened, the oxygen side space 1 can be communicated with the outside, a hydrogen side stop valve 41 on a hydrogen side discharge pipe 4 communicated with the hydrogen side space 2 is opened, and the hydrogen side space 2 can be communicated with the outside.
Step two: adding an electrolyte: electrolyte is added into the inner cavity of the container until the electrolyte is immersed in the comparison diaphragm, and the height of the electrolyte in the oxygen side space and the height of the electrolyte in the hydrogen side space are kept the same because the electrolyte can flow through the diaphragm, in the embodiment, the oxygen gas inlet valve 12 on the oxygen side gas inlet pipe 11 communicated with the oxygen side space 1 is opened, or the hydrogen gas inlet valve 22 on the hydrogen side gas inlet pipe 21 communicated with the hydrogen side space 2 is opened, and the electrolyte is added.
Step three: introducing gas: in this step, since hydrogen gas continuously enters the hydrogen side space 2 through the hydrogen side intake pipe 11 communicating with the hydrogen side space, even if the hydrogen side stop valve 41 is fully opened, the pressure in the hydrogen side space 2 is greater than the normal pressure (0.1 MPa), the pressure in the hydrogen side space 2 is controlled to be less than 0.2MPa, the pressure in the oxygen side space 1 is not less than the pressure in the hydrogen side space 2, and the pressure difference between both sides is less than 0.1kPa, because the hydrogen gas continuously enters the hydrogen side space 2 through the hydrogen side intake pipe 11 communicating with the hydrogen side space, the oxygen gas intake valve 12 is opened to allow oxygen gas to enter the electrolyte in the oxygen side space 1 through the oxygen side intake pipe 11, and the flow of the hydrogen gas entering the hydrogen side space 2 is controlled to be 2 times the flow of the oxygen gas entering the oxygen side space 1.
Step four: and (3) boosting test: keeping the flow rate of hydrogen entering the hydrogen side space 2 to be 2 times of the flow rate of oxygen entering the oxygen side space 1, controlling the opening degrees of the oxygen side stop valve 31 and the hydrogen side stop valve 41 to enable the pressure in the oxygen side space 1 and the hydrogen side space 2 to gradually rise, after the pressure in the hydrogen side space 2 reaches 0.2MPa, stably operating for 5-15 min under the state, detecting the content of hydrogen in the gas in the oxygen side discharge pipe 3 under the state and recording the content of oxygen in the gas in the A0.2 and the content of oxygen in the gas in the hydrogen side discharge pipe 4 and recording the content of oxygen in the gas in the oxygen side discharge pipe 3 and the content of oxygen in the hydrogen side discharge pipe 4 under the state and recording the data respectively according to the sequence after stably operating for 5-15 min under the state every time when the pressure in the hydrogen side space 2 rises to a set pressure value, and finally respectively recording the pressure in the hydrogen side space 2 to 3.2MPa, and after the stable operation is carried out for 5-15 min under the state, detecting the content of hydrogen in the gas in the oxygen side discharge pipe 3 under the state and marking as A3.2, and the content of oxygen in the gas in the hydrogen side discharge pipe 4 and marking as B3.2. Obviously, through the above-described operation procedure, the data of the content of hydrogen in the gas in the oxygen-side discharge pipe 3 will form a set of data a0.2 to a3.2, and the data of the content of oxygen in the gas in the hydrogen-side discharge pipe 4 will form a set of data B0.2 to B3.2, and for convenience of description, the set of data a0.2 to a3.2 will be referred to as an oxygen-side comparison data set, and the set of data B0.2 to B3.2 will be referred to as a hydrogen-side comparison data set. During the pressure increase, the pressure in the oxygen side space 1 is maintained at not less than the pressure in the hydrogen side space 2, and the pressure difference therebetween is maintained at less than 0.1 kPa.
Step five: and (3) parallel testing: dismantling the diaphragms used for comparison in the container, installing the diaphragms to be detected which are soaked in the electrolyte into the container, vertically arranging the diaphragms to be detected, dividing the inner cavity of the container into an oxygen side space 1 and a hydrogen side space 2, repeating the steps of adding the electrolyte and the step of three-way gas in the second step, and then performing the step of boosting the pressure in the fourth step, wherein the difference is that: in the boost test step, two situations can occur: the first one is: in the process of gradually increasing the pressure, when the pressure is increased to a certain pressure value (generally, when a diaphragm to be detected is detected, the pressure value can reach more than 1.0 MPa), if the content of hydrogen in the gas in the oxygen side discharge pipe 3 is detected to exceed a set value, or the content of oxygen in the gas in the hydrogen side discharge pipe 4 is detected to exceed a set value, recording the pressure value at the moment, and ending the test, wherein the condition indicates that the diaphragm to be detected can only be used within a safe working pressure range which is less than the pressure value, and under the condition, the content data of hydrogen in the gas in a group of oxygen side discharge pipes and the content data of oxygen in the gas in a group of hydrogen side discharge pipes of the diaphragm to be detected within the safe working pressure range can be sequentially recorded and obtained; the second method is as follows: in the process of gradually increasing the pressure, the measured content of hydrogen in the gas in the oxygen side discharge pipe 3 or the measured content of oxygen in the gas in the hydrogen side discharge pipe 4 does not exceed a set value, the content of hydrogen in the gas in the oxygen side discharge pipe 3 is detected and recorded as C3.2, the content of oxygen in the gas in the hydrogen side discharge pipe 4 is recorded and recorded as D3.2 after the pressure in the hydrogen side space 2 reaches 3.2MPa and is kept for 5-15 min, and the test is finished, wherein the condition shows that the diaphragm to be detected can be used within the pressure range of 0.1-3.2 MPa, and in this case, the content data of hydrogen in the gas in a group of oxygen side discharge pipes 3 can be recorded and recorded as C0.2-C3.2, and the content data of oxygen in the gas in a group of hydrogen side discharge pipes 4 can be recorded and recorded as D0.2-D3.2 in sequence. For convenience of description, the data of the content of hydrogen in the gas in the oxygen-side discharge pipe 3 obtained during the parallel test is referred to as an oxygen-side data group to be measured, and the data of the content of oxygen in the gas in the hydrogen-side discharge pipe 4 is referred to as a hydrogen-side data group to be measured.
Step six: and (3) comparative analysis: comparing the oxygen side to-be-tested data set and the hydrogen side to-be-tested data set of the diaphragm to be tested obtained in the parallel test with the oxygen side comparison data set and the hydrogen side comparison data set of the diaphragm to be compared obtained in the third step and the fourth step one by one, wherein the specific method comprises the following steps: if the second condition occurs in the step of boosting test of the diaphragm to be tested, a group of data groups to be tested on the oxygen side of C0.2-C3.2 and a group of data groups to be tested on the hydrogen side of D0.2-D3.2 are formed; when each data in the group C is smaller than the corresponding data in the group A and each data in the group D is smaller than the corresponding data in the group B, the fact that the air tightness of the diaphragm to be detected in the pressure range of 0.2-3.2 MPa is better than that of the diaphragm for comparison shows that the diaphragm to be detected can be used in a water electrolysis hydrogen production device with two rated pressures of 1.6MPa and 3.2MPa and can also be used in a water electrolysis hydrogen production device with variable pressure, and the purity of the generated hydrogen and oxygen is higher; when each data in the front section of the group C is smaller than the corresponding data in the front section of the group A, each data in the rear section of the group C is larger than the corresponding data in the rear section of the group A, each data in the front section of the group D is smaller than the corresponding data in the front section of the group B, each data in the rear section of the group D is larger than the corresponding data in the rear section of the group B, for example, each data in the groups C0.2-C2.0 is smaller than the corresponding data in the groups A0.2-A2.0, each data in the groups D0.2-D2.2 is smaller than the corresponding data in the groups B0.2-B2.2, each data in the groups C2.1-C3.2 is larger than the corresponding data in the groups A2.1-A3.2, and each data in the groups D2.3-D3.2 is larger than the corresponding data in the groups B2.3-B3.2, the gas tightness of the membrane to be detected in the pressure range of the groups A2-A3.2 is better than the gas tightness of the membrane for comparison, the water electrolysis device for producing hydrogen with a rated pressure of 1.6MPa, so that the oxygen gas is generated by water electrolysis; if the first condition occurs in the step of the pressure-increasing test of the diaphragm to be detected, the detected data group to be detected on the oxygen side and the detected data group to be detected on the hydrogen side within the safe working pressure range of the diaphragm to be detected are compared with the corresponding data of the comparison diaphragm within the safe working pressure range one by one, and the comparison and analysis method is the same as that of the second condition.
In the embodiment, when the pressure in the hydrogen side space 2 is increased from 0.2MPa to 3.2MPa, the set pressure value is 0.1MPa, namely, every time the pressure in the hydrogen side space 2 is increased by 0.1MPa, the content of hydrogen in the gas in the oxygen side discharge pipe 3 and the content of oxygen in the gas in the hydrogen side discharge pipe 4 are detected after the stable operation is carried out for 10min under the state, and data are recorded in sequence, finally, until the pressure in the hydrogen side space 2 reaches 3.2MPa, after the stable operation is carried out for 10min under the state, the content of hydrogen in the gas in the oxygen side discharge pipe 3 and the content of oxygen in the gas in the hydrogen side discharge pipe 4 under the state are detected, enough data can be collected by adopting the method, the gas tightness of the diaphragm to be detected and the diaphragm used for comparison can be comprehensively reflected after the comparison analysis, so that whether the diaphragm to be detected can be used in the hydrogen production water electrolysis device with rated pressure or variable pressure can be judged, thereby improving the purity of the hydrogen and oxygen produced by the water electrolysis hydrogen production device. In this embodiment, before installing the diaphragm in the first and fifth steps, the diaphragm to be compared or the diaphragm to be detected may be soaked in the electrolyte for 24 hours to be soaked in the electrolyte, and then installed, so that the electrolyte may smoothly flow through the diaphragm.
In step five in the present embodiment, the set value of the content of hydrogen in the gas in the oxygen-side discharge pipe 3 and the set value of the content of oxygen in the gas in the hydrogen-side discharge pipe 4 are both 2%.
In the present embodiment, for convenience of description, the ends of the oxygen-side discharge pipe 3 and the hydrogen-side discharge pipe 4 close to the container are referred to as the front ends, and the ends communicating with the outside are referred to as the ends. In order to facilitate the detection of the content of hydrogen in the gas in the oxygen-side discharge pipe 3 and the content of oxygen in the gas in the hydrogen-side discharge pipe 4, an oxygen-side detection pipe 5 is connected to the oxygen-side discharge pipe 3 at the front end of the oxygen-side cut-off valve 31, an oxygen detection valve 51 and a hydrogen content analyzer 52 are provided on the oxygen-side detection pipe 5, a hydrogen-side detection pipe 6 is connected to the hydrogen-side discharge pipe 4 at the front end of the hydrogen-side cut-off valve 41, and a hydrogen detection valve 61 and an oxygen content analyzer 62 are provided on the hydrogen-side detection pipe 6. The container is also provided with an oxygen side pressure transmitter 13 for detecting the pressure in the oxygen side space 1 and a hydrogen side pressure transmitter 23 for detecting the pressure in the hydrogen side space 2, the oxygen side stop valve 31 and the hydrogen side stop valve 41 are all electric regulating valves, the oxygen side pressure transmitter 13, the hydrogen side pressure transmitter 23, the oxygen side stop valve 31, the hydrogen side stop valve 41, the hydrogen content analyzer 52 and the oxygen content analyzer 62 are all in electric signal connection with the controller, so that the pressure in the oxygen side space 1 and the hydrogen side space 2 can be conveniently controlled, the pressure difference at two sides can be kept within an allowable range, the pressure is gradually increased from 0.2MPa to 3.2MPa, and the operation of increasing the pressure for 10min is kept every time the pressure is increased by 0.1 MPa.
In this embodiment, after the second step, since there is air remaining in the container and the pipes, the air in the container and the pipes can be replaced by nitrogen, so that the reaction of oxygen gas introduced into the oxygen-side space 1, hydrogen gas introduced into the hydrogen-side space 2 and the remaining air in the third step can be prevented. After the nitrogen replacement is completed, the gas is again introduced so that the oxygen side stop valve 31 and the hydrogen side stop valve 41 are kept fully open for a certain period of time, typically 5min, so that the nitrogen in the container and each pipe is replaced and the next operation is performed.
When the airtightness performance of the membrane is measured by the membrane airtightness measuring method, the pressure in the oxygen side space 1 is slightly higher than the pressure in the hydrogen side space 2, but the difference in pressure between the oxygen side space 1 and the hydrogen side space 2 is not more than 0.1 kPa. The oxygen side pressure transmitter 13 and the hydrogen side pressure transmitter 23 feed the measured results back to the controller in time, and then the controller controls the oxygen side stop valve 31 and the hydrogen side stop valve 41 to adjust the differential pressure until the adjustment is completed, and these steps require a certain time, usually about 15S. Therefore, the pressure difference between the oxygen side and the hydrogen side to be adjusted is set to a small value, usually 0.05 kPa, and when the controller detects that the pressure difference between the oxygen side and the hydrogen side is greater than 0.05 kPa by the oxygen side pressure transmitter 13 and the hydrogen side pressure transmitter 23, the controller controls the oxygen side stop valve 31 and the hydrogen side stop valve 41 to automatically adjust the opening degrees, so that the pressure difference between the oxygen side and the hydrogen side does not exceed 0.1 kPa.
In the embodiment, in order to facilitate the installation of the diaphragm and better simulate the actual working condition of the diaphragm in the water electrolysis hydrogen production device, the container comprises an oxygen side container and a hydrogen side container, the oxygen side container and the hydrogen side container are both pipes with one ends closed and the other ends opened, and the oxygen side container and the hydrogen side container are both horizontally placed. In actual manufacturing, the connecting flanges are arranged at the openings of the oxygen side container and the hydrogen side container, so that the oxygen side container and the hydrogen side container with the structure are easy to manufacture, can bear certain pressure and are convenient for the sealed butt joint of the oxygen side container and the hydrogen side container. During installation, the diaphragm is vertically arranged and clamped between the opening of the oxygen side container and the opening of the hydrogen side container, the opening of the oxygen side container is in sealed butt joint with the opening of the hydrogen side container, the diaphragm separates the inner cavity of the oxygen side container from the inner cavity of the hydrogen side container, the inner cavity of the oxygen side container is an oxygen side space 1, and the inner cavity of the hydrogen side container is a hydrogen side space 2.
In this embodiment, in order to allow oxygen gas entering the oxygen side space 1 to enter the electrolyte and then to exit through the oxygen side exhaust 3, the outlet end of the oxygen side intake tube 11 extends into the bottom of the oxygen side space 1. Likewise, in order to cause the hydrogen gas introduced into the hydrogen-side space 2 to enter the electrolyte and then to be discharged through the hydrogen-side discharge pipe 4, the outlet end of the hydrogen-side gas inlet pipe 21 protrudes into the bottom of the hydrogen-side space 2.
The invention has the advantages that: the air tightness detection method of the diaphragm simulates the working condition of the diaphragm in the water electrolysis hydrogen production device, can detect the pressure range applicable to the diaphragm to be detected, and can judge the quality of the air tightness of the diaphragm to be detected and the air tightness of the diaphragm used for comparison through parallel experiments, so that whether the diaphragm to be detected can be used in the water electrolysis hydrogen production device with rated pressure or variable pressure can be judged, and the purity of the hydrogen and oxygen produced by the water electrolysis hydrogen production device is further improved.
Claims (9)
1. The air tightness detection method of the diaphragm is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: installation: installing a diaphragm for comparison in a water electrolysis hydrogen production device with rated pressure of 1.6MPa and 3.2MPa in a closed container, vertically arranging the diaphragm for comparison, dividing the inner cavity of the container into an oxygen side space and a hydrogen side space, opening an oxygen side stop valve on an oxygen side discharge pipe communicated with the oxygen side space, wherein the oxygen side space can be communicated with the outside, opening a hydrogen side stop valve on a hydrogen side discharge pipe communicated with the hydrogen side space, and the hydrogen side space can be communicated with the outside;
step two: adding an electrolyte: adding electrolyte into the inner cavity of the container until the electrolyte submerges the diaphragm for comparison;
step three: introducing gas: oxygen enters electrolyte in the oxygen side space through an oxygen side gas inlet pipe communicated with the oxygen side space, hydrogen enters electrolyte in the hydrogen side space through a hydrogen side gas inlet pipe communicated with the hydrogen side space, and the flow of the hydrogen entering the hydrogen side space is controlled to be 2 times of the flow of the oxygen entering the oxygen side space; in the step, the pressure in the hydrogen side space is controlled to be more than the normal pressure and less than 0.2MPa, the pressure in the oxygen side space is not less than the pressure in the hydrogen side space, and the pressure difference between the two sides is less than 0.1 kPa;
step four: and (3) boosting test: controlling the opening degree of the oxygen side stop valve and the hydrogen side stop valve to enable the pressure in the oxygen side space and the hydrogen side space to gradually rise, keeping the pressure in the oxygen side space not less than the pressure in the hydrogen side space and the pressure difference between the two sides less than 0.1kPa in the pressure rising process, after the pressure in the hydrogen side space reaches 0.2MPa, stably operating for 5-15 min in the state, detecting the content of hydrogen in the gas in the oxygen side discharge pipe and the content of oxygen in the gas in the hydrogen side discharge pipe in the state, recording data, then controlling the pressure to continuously rise, and detecting the content of hydrogen in the gas in the oxygen side discharge pipe and the content of oxygen in the gas in the hydrogen side discharge pipe in the state after the pressure in the hydrogen side space rises upwards for a set pressure value every time, stably operating for 5-15 min in the state, and recording the data respectively according to sequence until the pressure in the hydrogen side space reaches 3.2MPa, After the stable operation is carried out for 5-15 min under the state, detecting the content of hydrogen in the gas in the oxygen side discharge pipe and the content of oxygen in the gas in the hydrogen side discharge pipe under the state and respectively recording the contents; thus, through the operation process, the content data of the hydrogen in the gas in the oxygen side discharge pipe can form an oxygen side comparison data set, and the content data of the oxygen in the gas in the hydrogen side discharge pipe can form a hydrogen side comparison data set;
step five: and (3) parallel testing: dismantling the diaphragms used for comparison in the container, installing the diaphragms to be detected in the container, vertically arranging the diaphragms to be detected, repeating the steps of adding electrolyte and three-way gas in the second step, and then performing the step-up test in the fourth step, wherein the difference lies in that: in the boost test step, two situations can occur: the first one is: in the process of gradually increasing the pressure, when the pressure is increased to a certain pressure value, if the content of hydrogen in the gas in the oxygen side discharge pipe is measured to exceed a set value or the content of oxygen in the gas in the hydrogen side discharge pipe is measured to exceed the set value, recording the pressure value at the moment, and ending the test, wherein the condition shows that the diaphragm to be detected can only be used in a safe working pressure range which is less than the pressure value; the second method is as follows: in the process of gradually increasing the pressure, the measured content of hydrogen in the gas in the oxygen side discharge pipe or the measured content of oxygen in the gas in the hydrogen side discharge pipe does not exceed a set value, the content of hydrogen in the gas in the oxygen side discharge pipe and the content of oxygen in the gas in the hydrogen side discharge pipe are detected and respectively recorded after the pressure in the hydrogen side space reaches 3.2MPa and the state is maintained for 5-15 min, and the test is finished, wherein the condition shows that the diaphragm to be detected can be used within the pressure range of 0.1-3.2 MPa; thus, through the parallel test process, the content data of the hydrogen in the gas in the oxygen side discharge pipe can form an oxygen side data group to be tested, and the content data of the oxygen in the gas in the hydrogen side discharge pipe can form a hydrogen side data group to be tested;
step six: and (3) comparative analysis: the specific method comprises the following steps: if the second condition occurs in the step-up test step of the diaphragm to be detected, when each data in the oxygen side to-be-detected data group is smaller than the corresponding data in the oxygen side comparison data group and each data in the hydrogen side to-be-detected data group is smaller than the corresponding data in the hydrogen side comparison data group, the fact that the air tightness of the diaphragm to be detected in the pressure range of 0.2-3.2 MPa is better than that of the diaphragm used for comparison shows that the diaphragm to be detected in the pressure range of 0.2-3.2 MPa can be used in a water electrolysis hydrogen production device with two rated pressures of 1.6MPa and 3.2MPa and can also be used in a water electrolysis hydrogen production device with variable pressure; when each datum in the front section of the oxygen side to-be-detected data set is smaller than a corresponding datum in the front section of the oxygen side comparison data set, each datum in the rear section of the oxygen side to-be-detected data set is larger than a corresponding datum in the rear section of the oxygen side comparison data set, and each datum in the front section of the hydrogen side to-be-detected data set is smaller than a corresponding datum in the front section of the hydrogen side comparison data set, and each datum in the rear section of the hydrogen side to-be-detected data set is larger than a corresponding datum in the rear section of the oxygen side comparison data set, the airtightness of the diaphragm to be detected in the front section pressure range corresponding to the front section datum is better than the airtightness of the diaphragm for comparison, and the diaphragm to be detected can be used in the water electrolysis hydrogen production device with rated pressure in the front section pressure range; if the first condition occurs in the step of the pressure-increasing test of the diaphragm to be detected, the detected oxygen side data group to be detected and the detected hydrogen side data group to be detected within the safe working pressure range of the diaphragm to be detected are compared with the corresponding data of the comparison diaphragm within the safe working pressure range one by one, and the comparison and analysis method is the same as that of the second condition.
2. The method for detecting the airtightness of a separator according to claim 1, wherein: in the fourth step, the set pressure value is 0.1 MPa.
3. The method for detecting the airtightness of a separator according to claim 1, wherein: in the fifth step, the set value of the hydrogen gas content in the gas in the oxygen-side discharge pipe and the set value of the oxygen gas content in the gas in the hydrogen-side discharge pipe are both 2%.
4. The method for detecting the airtightness of a separator according to claim 1, wherein: the oxygen side discharge pipe at the front end of the oxygen side stop valve is communicated with an oxygen side detection pipe, the oxygen side detection pipe is provided with an oxygen detection valve and a hydrogen content analyzer, the hydrogen side discharge pipe at the front end of the hydrogen side stop valve is communicated with a hydrogen side detection pipe, the hydrogen side detection pipe is provided with a hydrogen detection valve and an oxygen content analyzer, the container is also provided with an oxygen side pressure transmitter for detecting the pressure in the oxygen side space and a hydrogen side pressure transmitter for detecting the pressure in the hydrogen side space, the oxygen side stop valve and the hydrogen side stop valve are electric regulating valves, the oxygen side pressure transmitter, the hydrogen side pressure transmitter, the oxygen side stop valve, the hydrogen content analyzer and the oxygen content analyzer are all in electric signal connection with the controller.
5. The method for detecting the airtightness of a separator according to claim 1, 2, 3 or 4, wherein: and D, soaking the diaphragm used for comparison in the step one and the diaphragm to be detected in the step five in the electrolyte for 24 hours, and then installing.
6. The method for detecting the airtightness of a separator according to claim 1, 2, 3 or 4, wherein: the container comprises an oxygen side container and a hydrogen side container, wherein the oxygen side container and the hydrogen side container are both pipes with one ends closed and the other ends opened; when the oxygen side container is installed, the membrane is vertically arranged and is clamped between the opening of the oxygen side container and the opening of the hydrogen side container, the opening of the oxygen side container is in sealed butt joint with the opening of the hydrogen side container, and the membrane separates the inner cavity of the oxygen side container from the inner cavity of the hydrogen side container.
7. The method for detecting the airtightness of a separator according to claim 6, wherein: the oxygen side container and the hydrogen side container are both horizontally placed.
8. The method for detecting the airtightness of a separator according to claim 1, 2, 3 or 4, wherein: the outlet end of the oxygen side gas inlet pipe extends into the bottom of the oxygen side space, and the outlet end of the hydrogen side gas inlet pipe extends into the bottom of the hydrogen side space.
9. The method for detecting the airtightness of a separator according to claim 1, 2, 3 or 4, wherein: and after the second step is finished, replacing the air in the container and each pipeline by nitrogen, and after the nitrogen replacement is finished, performing the operation of the third step.
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| CN202111585856.6A CN114486079A (en) | 2021-12-23 | 2021-12-23 | Air tightness detection method of diaphragm |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116426974A (en) * | 2023-03-03 | 2023-07-14 | 浙江蓝能氢能科技股份有限公司 | Gas permeation system and testing method of electrolytic hydrogen production device |
| CN117968988A (en) * | 2024-04-02 | 2024-05-03 | 北京英博新能源有限公司 | Air tightness detection device of PEM (PEM) electrolytic tank |
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2021
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116426974A (en) * | 2023-03-03 | 2023-07-14 | 浙江蓝能氢能科技股份有限公司 | Gas permeation system and testing method of electrolytic hydrogen production device |
| CN117968988A (en) * | 2024-04-02 | 2024-05-03 | 北京英博新能源有限公司 | Air tightness detection device of PEM (PEM) electrolytic tank |
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