CN217901489U - Bi-component gas separation testing device - Google Patents

Bi-component gas separation testing device Download PDF

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CN217901489U
CN217901489U CN202123035953.6U CN202123035953U CN217901489U CN 217901489 U CN217901489 U CN 217901489U CN 202123035953 U CN202123035953 U CN 202123035953U CN 217901489 U CN217901489 U CN 217901489U
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gas
component
membrane
gas cylinder
way valve
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陈秋霞
贾明民
肖慧芳
赵宜江
李梅生
周守勇
任梦媛
刘苗苗
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Huaiyin Normal University
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Abstract

The utility model relates to a bi-component gas separation testing arrangement belongs to gas separation technical field. The method comprises the following steps: the first gas cylinder and the second gas cylinder are respectively connected with the interception side of the membrane component through a first mass flow meter and a second mass flow meter; the membrane component is used for separating the mixed gas obtained from the first gas cylinder and the second gas cylinder; a purge gas cylinder connected to the permeate side of the membrane module for supplying a purge gas to the permeate side; further comprising: and the gas chromatograph and the flowmeter are connected to the permeation side of the membrane component and are used for detecting the composition and the flow of the gas obtained from the permeation side. The gas permeation testing device of the utility model can be used for configuring mixed gas with different proportions and researching the gas permeation performance of the mixed component under certain temperature, pressure and temperature; meanwhile, residue removal treatment can be performed in the equipment after the test is finished.

Description

Bi-component gas separation testing device
Technical Field
The utility model relates to a bi-component gas separation testing arrangement belongs to gas separation technical field.
Background
The membrane separation is a new separation technology which appears at the beginning of the 20 th century and rises rapidly after the 60 s of the 20 th century, and the membrane separation technology has the functions of separation, concentration, purification and refining, and has the characteristics of high efficiency, energy conservation, environmental protection, simple molecular filtration and filtration process, easy control and the like, so the membrane separation technology is widely applied to the fields of food, medicine, biology, environmental protection, chemical industry, metallurgy, energy, petroleum, water treatment, electronics, bionics and the like at present, generates huge economic benefit and social benefit, and becomes one of the most important means in the separation science at present.
The permeability coefficient is a measure of the ease with which a gas passes through the membrane, and a smaller permeability coefficient is better for a sealing material, and a larger permeability coefficient is better for a gas separation membrane. The separation coefficient indicates the separation capacity of the membrane for different gases, and the larger the separation coefficient, the easier the gas is separated.
The principle of gas permeability coefficient measurement is to divide a measured sheet sample into two spaces. The gas amount permeated was measured with a detector, one being the gas supply side at a higher pressure and one being the permeate side at a lower pressure. The so-called gas permeability coefficient is the product of the amount of gas that permeates through a unit area per unit time and unit pressure and the thickness of the sample.
The measurement of the gas permeability coefficient is classified into a pressure method and a volume method. The pressure method is a method in which a change in pressure is detected by a vacuum gauge under a constant volume on the permeation side, and a differential pressure method is generally usedThe instrument for measuring the gas permeability coefficient has limited range of the measured gas permeability coefficient because the volume of the permeation side is fixed, and cannot test the permeability of the mixed gas because no detectors such as a mass analyzer, a gas chromatograph and the like are connected; the volume method is a method in which when the pressure at the permeate side is constant (the pressure at the permeate side is generally maintained at 1 atm), the volume change is measured by a detector, and the method can be used for O 2 、CO 2 Coexistence of moisture and measurement of mixed gas. Therefore, designing a high-efficiency and accurate volumetric gas separation device becomes a bottleneck of research.
SUMMERY OF THE UTILITY MODEL
The utility model discloses the first technical problem that will solve is: the separation performance of the bi-component gas in the membrane separation process is tested, and the test process needs to be more convenient and accurate. In the device that this patent adopted, through setting up two kinds of air supplies to controllable regulation through the flowmeter, realize testing the purpose of aassessment to membrane separation process under the different air supply component circumstances.
The utility model discloses the second technical problem that will solve is: in the equipment with the humidifying system, when residual gas removal operation is required after the test is finished, water in the heating equipment in the pipeline is easily pumped out when vacuum pumping operation is carried out, so that the residual gas removal effect is poor. This patent is through specific pipeline design, has bypassed humidification equipment, can realize also carrying out the desorption to the residual gas in the feed line.
The technical scheme is as follows:
a two-component gas separation test apparatus comprising:
the first gas cylinder and the second gas cylinder are respectively connected with the interception side of the membrane component through a first mass flow meter and a second mass flow meter;
the membrane component is used for separating the mixed gas obtained from the first gas cylinder and the second gas cylinder;
a purge gas cylinder connected to the permeate side of the membrane module for supplying a purge gas to the permeate side;
further comprising: and the gas chromatograph and the flowmeter are connected to the permeation side of the membrane component and are used for detecting the composition and the flow of the gas obtained from the permeation side.
Further comprising: the membrane component comprises a first humidification tank and a second humidification tank which are sequentially connected in series, wherein the first gas cylinder and the second gas cylinder are connected to the interception side of the membrane component through the first humidification tank and the second humidification tank, and the first humidification tank and the second humidification tank are used for humidifying gas.
The first gas cylinder and the second gas cylinder are both connected to the first humidifying tank through a first tee joint, and the second humidifying tank is connected to the interception side of the membrane component through a third tee joint; and the first three-way valve and the third three-way valve are also connected.
Further comprising: and the vacuum pump is respectively connected with the permeation side of the membrane component and the third three-way valve through a second three-way valve.
In one embodiment, the first mass flow meter and the second mass flow meter are connected to the interception side of the membrane module through a first tee joint.
In one embodiment, the gas chromatograph and flow meter is connected to the permeate side of the membrane module by a fourth three-way valve.
In one embodiment, a back pressure valve and a pressure gauge are also connected to the retentate side of the membrane module.
In one embodiment, a first gas cylinder is connected to the retentate side of the membrane module through a first filter; the second gas cylinder is connected with the interception side of the membrane component through a second filter; the purging gas cylinder is connected with the interception side of the membrane module through a third filter.
In one embodiment, the membrane module is placed in a constant temperature oven.
Advantageous effects
Because the gas permeation testing device of the utility model comprises the mass flow meter, the humidifying tank, the temperature control box, the back pressure valve, the purging mechanism and the gas chromatography device, mixed gas with different proportions can be configured during use, and the gas permeation performance of mixed components can be rapidly and accurately tested under certain temperature, pressure and temperature; meanwhile, residue removal treatment can be performed in the equipment after the test is finished.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a view of the structure of the apparatus of the present invention;
wherein, 1, a first gas cylinder; 2. a second gas cylinder; 3. purging the gas cylinder; 4. a first pressure reducing valve; 5. a second pressure reducing valve; 6. a third pressure reducing valve; 7. a first mass flow meter; 8. a second mass flow meter; 9. a third mass flow meter; 10. a first filter; 11. a second filter; 12. a third filter; 13. a first tee joint; 14. a first three-way valve; 15. a second three-way valve; 16. a first humidification tank; 17. a second humidification tank; 18. a third three-way valve; 19. a needle valve; 20. a constant-temperature oven; 21. a membrane module; 22. a pressure gauge; 23. a back pressure valve; 24. a fourth three-way valve; 25. gas chromatography; 26. a flow meter; 27. a fifth three-way valve; 28. a second tee joint; 29. a vacuum pump.
Detailed Description
As shown in fig. 1, the separation testing apparatus in this patent is mainly composed of seven modules, which are respectively: the device comprises a gas configuration mechanism, a gas humidification mechanism, a gas separation mechanism, a membrane module pressure control mechanism, a membrane flux and selectivity testing mechanism, a purge gas control mechanism and a residue removal mechanism.
The gas configuration mechanism is used for premixing the two-component gas and adjusting corresponding gas state parameters for subsequent separation and test processes;
the gas humidifying mechanism is used for heating the gas obtained in the gas configuration mechanism so as to be suitable for the subsequent membrane separation process;
the gas separation mechanism mainly comprises a separation membrane used for separating and treating the two-component gas;
the membrane flux and selectivity testing mechanism is used for detecting the flow and the content of the gas obtained by separation in the gas separation mechanism so as to achieve the purpose of detecting the membrane separation process;
a purge gas control means for supplying a purge gas to the permeate side of the separation membrane to separate the separated component from the separation membrane;
the residue removing mechanism is used for removing residual gas in the device.
More specifically, the structure is as follows:
the gas configuration device comprises a first gas bottle 1 and a second gas bottle 2 which are respectively used for storing two different gases, and are respectively connected with a first mass flow meter 7 and a second mass flow meter 8 through a first pressure reducing valve 4 and a second pressure reducing valve 5, and the downstream sections of the gas configuration device are respectively connected with a first filter 10 and a second filter 11 which are respectively used for filtering the gases and protecting the separation membrane; and then is connected to the first tee 13 at the same time to realize the mixing of the two gases; then is connected with a subsequent gas humidifying mechanism;
the gas humidifying mechanism comprises a first humidifying tank 16 and a second humidifying tank 17, the first humidifying tank 16 and the second humidifying tank 17 receive the mixed gas obtained by the first tee joint 13 and perform humidifying treatment, the gas obtained by the first tee joint 11 is connected with the first humidifying tank 16 through a first three-way valve 14, the outlet of the second humidifying tank 17 is connected with a second three-way valve 15, and the first three-way valve 14 is simultaneously connected with the second three-way valve 15; in addition, the second three-way valve 15 is connected to the cut-off side of the membrane module 21 and the vacuum pump 29 through the third three-way valve 18, respectively; the membrane module 2 is used for separating gas, and the vacuum pump 29 is used for removing residual gas in the pipeline.
The gas separation mechanism comprises an oven and a membrane module 21, the membrane module 21 is divided into an interception side and a permeation side through a separation membrane and is used for separating two-component gas, in the separation process, the intercepted gas is left on the interception side, the permeated gas enters the permeation side, the interception side is also connected with a backpressure valve 23, the interception side is also connected with a pressure gauge 22, and the pressure of the interception side, namely the separation pressure, is regulated and controlled through the backpressure valve 23; the permeation side is also respectively connected with a gas chromatograph 25 and a flow meter 27 through a fourth three-way valve 24, so that the permeation amount and the gas composition of the gas on the permeation side can be detected; the membrane assembly 21 is positioned in the constant-temperature oven 20;
the purging gas control mechanism comprises a purging gas cylinder 3, a third pressure reducing valve 6 and a third filter 12 which are connected in sequence; connected to the permeate side of the membrane module 21 by a fifth three-way valve 27 for feeding a sweep gas to the permeate side during the separation;
for the residue removing mechanism, a vacuum pump 29 is included, which is connected with the fifth three-way valve 27 and the third three-way valve 18 through a second three-way valve 28; the evacuation operation may be performed while simultaneously evacuating the membrane module 21 and the residual gas in a series of lines in the permeate side and the retentate side. Specifically, the first gas cylinder 1 and the second gas cylinder 2 are both connected to a first humidification tank 16 through a first three-way valve 13, and a second humidification tank 17 is connected to the retentate side of a membrane module 21 through a third three-way valve 18; and a connection is made between the first three-way valve 13 and the third three-way valve 18. Further comprising: and a vacuum pump 29 connected to the permeate side of the membrane module 21 and the third three-way valve 18 through a second three-way valve 28. Because the vacuum pumping process is needed during the residue removing operation, if a humidifying device is arranged in the pipeline, water in the pipeline is easy to be pumped out, through the pipeline design, when the vacuum pump 29 is started, the second filter 11, the first three-way valve 14, the second three-way valve 15 and the third three-way valve 18 are communicated through the opening and closing process of the three-way valves, the first humidifying tank 16 and the second humidifying tank 17 can be bypassed, and residual gas in the raw gas pipeline can be pumped out.
The pipelines in the gas permeation testing device are all 1/8inch316 stainless steel pipes and mass flowmeters (CO) 2 ) 7 mass flow meter 8 (N) 2 ) And the flow control range of the mass flow meter 9 (Ar or He) is 0-100ml/min, wherein the tee joint, the four-way joint, the diaphragm valve and the ball valve are all ferrule type interfaces, and the design pressure is 0-2.5Mpa.
The utility model discloses a test principle as follows:
the utility model discloses a measurement principle is based on the formula:
Figure BDA0003393557100000041
wherein, P-permeability coefficient, selective layer thickness (cm) of L-membrane, N i Volume flow (cm) of the i component 3 Pers), limited test area (cm) of A-membranes 2 ),Δp i Transmembrane pressure difference (cmHg).
The utility model discloses utilize 1, first gas cylinder, second gas cylinder 2, sweep gas cylinder 3 and affiliated manometer control feeding side total pressure, utilize the ratio of first mass flow meter 7 and the 8 control mixing gas of second mass flow meter, utilize the flow of the 9 control purge gas of third mass flow meter, utilize gas chromatography 25 to test the gaseous constitution of infiltration side, utilize flowmeter 26 (soap bubble flowmeter or rotor flowmeter) to test infiltration side gas flow, utilize vacuum pump 29 to get rid of membrane feeding side and infiltration side residual gas, realize the accurate high-efficient test of device.
The utility model discloses a test operation process as follows:
the first step is as follows: sample installation and systematic disablement
a) Preparing a sample, placing the membrane sample in the membrane module 21, and sealing with a rubber ring;
b) Confirming that the sample is placed, installing a membrane assembly cover plate, and screwing down screws;
c) Opening the needle valve 19, closing the backpressure valve 23, closing the fourth three-way valve 24, switching the outlet end of the third three-way valve 18 downwards, and switching the outlet end of the fifth three-way valve 27 downwards;
d) And starting a vacuum pump 29 to ensure that the upper side and the lower side of the membrane component are sealed, vacuumizing for more than half an hour to ensure that residual air in the system and dissolved gas in the sample are removed.
The second step: membrane module raw material side mixed gas blending and pressure control
a) Closing the first pressure reducing valve 4 and the second pressure reducing valve 5;
b) Opening the first gas cylinder 1 and the second gas cylinder 2, and regulating and controlling the pressure of the pressure reducing valve within the range of 0-2.5 MPa;
c) Opening the first pressure reducing valve 4 and the second pressure reducing valve 5, regulating and controlling the flow of the first mass flowmeter 7 and the flow of the second mass flowmeter 8, and regulating the proportion of the mixed gas;
d) Switching the outlet port of the first three-way valve 14 to the left side, switching the outlet port of the second three-way valve 15 to the right side, switching the outlet port of the third three-way valve 18 to the upper side, opening the needle valve 19, and roughly adjusting the film supply side pressure;
e) And adjusting a back pressure valve 23, observing the pressure of a pressure gauge 22, and adjusting the pressure range to be 0-2.5MPa.
The third step: membrane module permeate side-blow scavenging control
a) The outlet end of the fifth three-way valve 27 is switched to the upper side, and the third reducing valve 6 is closed;
b) Adjusting the pressure of the purging gas cylinder 3 to be within the range of 0-2.5 MPa;
c) Opening a third pressure reducing valve 6, and regulating and controlling the flow of a third mass flowmeter 9;
the fourth step: control of ambient temperature and humidity for membrane testing
a) The outlet end of the third three-way valve 18 is switched to the upper side, and the outlet end of the fifth three-way valve 27 is switched to the upper side;
b) Opening the membrane module 21 and placing the membrane sample;
c) Opening the switch of the constant temperature oven 20, and adjusting the temperature of the oven to the testing temperature
d) And (3) adjusting humidity: and switching the outlet end of the first three-way valve 14 to the right side and switching the outlet end of the second three-way valve 15 to the left side to perform humidification treatment on the gas separation membrane.
The fifth step: membrane flux and selectivity testing
a) And (3) membrane flux test: the outlet end of the fourth three-way valve 24 is switched to the lower side, the gas flow on the permeation side of the membrane is tested by using the flowmeter 26, and the membrane flux is calculated by using a formula.
b) And (3) membrane selectivity test: the outlet end of the fourth three-way valve 24 was switched to the upper side, and the gas selectivity was tested by means of a gas chromatograph 25.
And a sixth step: sample removal
a) Closing the first gas cylinder 1, the second gas cylinder 2 and the purging gas cylinder 3;
b) Opening the membrane module 21 and taking out the test sample;
c) Finally, the residual gum on the surface of the sample stage is removed, preferably with acetone or methanol.
Preferably, the first use can be started directly from the second step.
The utility model discloses can also measure the gas permeability coefficient of materials such as film, sheet, high resistant barrier material and metal foil.

Claims (9)

1. A two-component gas separation test apparatus, comprising:
the first gas cylinder (1) and the second gas cylinder (2) are respectively connected with the interception side of the membrane component (21) through a first mass flow meter (7) and a second mass flow meter (8);
the membrane component (21) is used for separating mixed gas obtained from the first gas cylinder (1) and the second gas cylinder (2);
a purge gas cylinder (3) connected to the permeate side of the membrane module (21) for supplying a purge gas to the permeate side;
further comprising: and a gas chromatograph (25) and a flow meter (26) connected to the permeate side of the membrane module (21) and used for detecting the composition and flow rate of the gas obtained from the permeate side.
2. The two-component gas separation test apparatus of claim 1, further comprising: the membrane component is characterized by comprising a first humidifying tank (16) and a second humidifying tank (17) which are connected in series in sequence, wherein the first gas cylinder (1) and the second gas cylinder (2) are connected to the interception side of the membrane component (21) through the first humidifying tank (16) and the second humidifying tank (17), and the first humidifying tank (16) and the second humidifying tank (17) are used for humidifying gas.
3. The two-component gas separation test unit according to claim 1, wherein the first gas cylinder (1) and the second gas cylinder (2) are connected to the first humidification tank (16) through a first three-way valve (13), and the second humidification tank (17) is connected to the retentate side of the membrane module (21) through a third three-way valve (18); and the first three-way valve (13) and the third three-way valve (18) are also connected.
4. The two-component gas separation test apparatus of claim 1, further comprising: and a vacuum pump (29) connected to the permeate side of the membrane module (21) and the third three-way valve (18) through a second three-way valve (28).
5. The two-component gas separation test device according to claim 1, wherein the first mass flow meter (7) and the second mass flow meter (8) are connected to the retentate side of the membrane module (21) through a first tee (13).
6. The two-component gas separation test unit according to claim 1, wherein the gas chromatograph (25) and the flow meter (26) are connected to the permeate side of the membrane module (21) through a fourth three-way valve (24).
7. The two-component gas separation test device according to claim 1, wherein a back pressure valve (23) and a pressure gauge (22) are further connected to the retentate side of the membrane module (21).
8. The two-component gas separation test device according to claim 1, wherein the first gas cylinder (1) is connected to the retentate side of the membrane module (21) through a first filter (10); the second gas cylinder (2) is connected with the interception side of the membrane component (21) through a second filter (11); the purging gas bottle (3) is connected with the interception side of the membrane component (21) through a third filter (12).
9. The two-component gas separation test unit according to claim 1, wherein the membrane module (21) is placed in a constant temperature oven (20).
CN202123035953.6U 2021-12-06 2021-12-06 Bi-component gas separation testing device Active CN217901489U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116148155A (en) * 2023-02-27 2023-05-23 贝士德仪器科技(北京)有限公司 Gas separation membrane permeability and separation coefficient tester and testing method thereof
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

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116148155A (en) * 2023-02-27 2023-05-23 贝士德仪器科技(北京)有限公司 Gas separation membrane permeability and separation coefficient tester and testing method thereof
CN116148155B (en) * 2023-02-27 2023-09-29 贝士德仪器科技(北京)有限公司 Gas separation membrane permeability and separation coefficient tester and testing method thereof
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

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