CN116148155B - Gas separation membrane permeability and separation coefficient tester and testing method thereof - Google Patents
Gas separation membrane permeability and separation coefficient tester and testing method thereof Download PDFInfo
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- CN116148155B CN116148155B CN202310169933.2A CN202310169933A CN116148155B CN 116148155 B CN116148155 B CN 116148155B CN 202310169933 A CN202310169933 A CN 202310169933A CN 116148155 B CN116148155 B CN 116148155B
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Abstract
The tester for the permeability and the separation coefficient of the gas separation membrane and the testing method thereof can adopt two principles of a steady state method and an unsteady state method to realize the test of the permeability and the separation coefficient of single-component or multi-component gas by the gas separation membrane, and simultaneously, the tester can be used for detecting the gas with weak permeability and separation capability after enriching, thereby improving the detection sensitivity.
Description
Technical Field
The invention relates to the field of instruments and equipment related to gas separation membrane testing, in particular to a tester for gas separation membrane permeability and separation coefficient and a testing method thereof.
Background
The gas separation membrane is a selectively permeable membrane, the mechanical strength of which can ensure the gas separation membrane to bear a certain pressure difference. Different gas separation membranes have different permeabilities (characterized by "permeabilities") and selectivities (characterized by "separation coefficients") for different types of gas molecules, and thus can selectively separate a gas from a gas mixture. Such as collecting oxygen from air, recovering hydrogen from synthesis ammonia tail gas, separating hydrogen, carbon monoxide, etc. from petroleum cracking gas mixtures. The apparatus and the device for evaluating and testing the permeability and the separation coefficient of the gas separation membrane are necessary tools for researching the gas separation membrane.
Disclosure of Invention
The technical scheme provided by the invention is as follows: the gas path structure of the gas separation membrane permeability and separation coefficient tester is divided into an upper part and a lower part by taking the gas separation membrane as a boundary, namely a gas path structure at the upper part of the gas separation membrane and a gas path structure at the lower part of the gas separation membrane.
The gas circuit structure on gas separation membrane upper portion includes: the air inlet of the first mass flow controller is connected with the air outlet of the first air source; the air inlet of the second mass flow controller is connected with the air outlet of the second air source; the air outlets of the first mass flow controller and the second mass flow controller are combined together and connected with the first interface of the first four-way valve; the gas separation membrane clamp comprises an upper cavity and a lower cavity, a gas separation membrane is clamped between the upper cavity and the lower cavity of the gas separation membrane clamp, both ends of the upper cavity and the lower cavity of the gas separation membrane clamp are respectively provided with a gas inlet and a gas outlet, the gas inlet of the upper cavity is connected with the fourth interface of the first four-way valve, and the gas outlet of the upper cavity is connected with the third interface of the first four-way valve; the first pressure sensor is fixedly arranged on a branch of a connecting pipeline between a fourth interface of the first four-way valve and an air inlet of the upper cavity of the gas separation membrane clamp; the second port of the first four-way valve is connected with the first port of the second four-way valve, and the second port of the second four-way valve is connected with the tail gas exhaust port; the gas inlet of the gas detector interface is connected with the fourth interface of the second four-way valve, the gas outlet of the gas detector interface is connected with the tail gas exhaust port, and the gas detector is connected to the gas detector interface.
The gas path structure at the lower part of the gas separation membrane comprises two optional structures, namely a steady-state method gas path structure or an unsteady-state method gas path structure.
The steady-state method gas circuit structure comprises: the air inlet of the third mass flow controller is connected with the air outlet of the third air source, the air outlet of the third mass flow controller is connected with the air inlet of the lower cavity of the gas separation membrane clamp, the air outlet of the lower cavity of the gas separation membrane clamp is connected with the third port of the second four-way valve, and the second pressure sensor is fixedly arranged on a branch of a connecting pipeline of the air outlet of the third mass flow controller and the air inlet of the lower cavity of the gas separation membrane clamp.
The unsteady state method gas circuit structure includes: an air inlet of the third mass flow controller is connected with an air outlet of a third air source, the air outlet of the third mass flow controller is connected with an interface IV of a third four-way valve, and an air inlet of a lower cavity of the air separation membrane clamp is connected with an air outlet of the air circulation pump; the gas outlet of the lower cavity of the gas separation membrane clamp is connected with the second port of the third four-way valve, the gas inlet of the gas circulation pump is connected with the first port of the third four-way valve, the second pressure sensor is fixedly arranged on the branch path of the gas inlet of the lower cavity of the gas separation membrane clamp and the connecting pipeline of the gas circulation pump, and the third port of the third four-way valve is connected with the third port of the second four-way valve.
Optionally, the upper cavity and the lower cavity of the gas separation membrane clamp have heating functions, and can be gas separation membrane heating treatment.
Optionally, a back pressure valve may be installed on a connection pipeline between the first four-way valve and the second four-way valve, an air inlet of the back pressure valve is connected with the second port of the first four-way valve, and an air outlet of the back pressure valve is connected with the first port of the second four-way valve.
Optionally, in the steady-state method gas path structure at the lower part of the gas separation membrane, a cold trap pipe is installed between the lower cavity of the gas separation membrane fixture and the second four-way valve, and the connection mode is as follows: the air inlet of the cold trap tube is connected with the air outlet of the lower cavity of the gas separation membrane clamp, the air outlet of the cold trap tube is connected with the third port of the second four-way valve, the cold trap tube is arranged in a cold trap cup, and liquid refrigerant is placed in the cold trap cup.
Alternatively, the gas detector may be a thermal conductivity detector, a mass spectrum detector, an infrared spectrum detector, or the like.
The permeability and separation coefficient testing method is a method for testing based on a gas separation membrane permeability and separation coefficient tester, and the testing method is divided into a steady state method and an unsteady state method:
Method one, steady state method:
the steady state method is a test method based on a tester consisting of a gas path structure of the steady state method in the structure of the upper part of the gas separation membrane and the optional two structures of the lower part of the gas separation membrane;
the steady state method test steps are as follows:
step one S01: a gas separation membrane activation pretreatment process comprising: the gas separation membrane with the area S is arranged on a gas separation membrane clamp, an upper cavity and a lower cavity of the gas separation membrane clamp heat the gas separation membrane to enable impurity gas adsorbed on the surface of the gas separation membrane to be desorbed, meanwhile, the second mass flow controller controls purge gas in a second gas source to flow out at a certain flow rate, and the first four-way valve is switched into a state that the first interface is communicated with the fourth interface, the second interface is communicated with the third interface, the first interface is isolated from the second interface, the third interface is isolated from the fourth interface, and the purge gas flowing out from the second mass flow controller flows out through the upper end of the gas separation membrane; the third mass flow controller controls the purge gas in the third gas source to flow out through the lower end of the gas separation membrane at a certain flow rate; the purging gas flowing through the upper end and the lower end of the gas separation membrane blows away the impurity gas desorbed by heating;
Step two S02: a gas permeation and separation process comprising: the gas separation membrane clamp stops heating to enable the gas separation membrane to return to room temperature, the second mass flow controller is closed, the first mass flow controller controls the test gas in the first gas source to flow out from the upper end of the gas separation membrane at a certain flow rate, the test gas is mixed gas with known concentration of each component, the permeation rate and separation coefficient test of two components in the mixed gas are described below, other components are similar, the two components are named as component 1 and component 2, and the molar concentration of the component 1 is C 11 Component 2 has a molar concentration of C 21 The method comprises the steps of carrying out a first treatment on the surface of the At this time, the first pressure sensor records that the gas pressure at the upper end of the gas separation membrane is P 1 The method comprises the steps of carrying out a first treatment on the surface of the The test gas component 1 and the component 2 at the upper end of the gas separation membrane penetrate into the lower end of the gas separation membrane through the gas separation membrane, and the second pressure sensor records that the pressure value of the lower end of the gas separation membrane is P 2 ；
Step S03: permeation and separation gas detection: the third mass flow controller controls the gas in the third gas source to blow the gas permeated from the upper end of the gas separation membrane to the lower end of the gas separation membrane to the interface of the gas detector, and the gas detector detects that the molar concentration of the component 1 in the flowing gas is C 12 Component 2 has a molar concentration of C 22 When the detection time period is t, the gas amount of the component 1 permeated from the upper end of the gas separation membrane to the lower end of the gas separation membrane is V 1 The gas amount of component 2 is V 2 ；
Step S04: and (3) calculating the permeability and the separation coefficient:
and (3) calculating the permeability: the permeability is the gas quantity of a certain component gas in the mixed gas at the upper end of the gas separation membrane (15) in unit time, unit pressure difference and unit cross section area of the gas separation membrane (15) entering the lower end of the gas separation membrane (15) in a permeation mode, and the calculation formula is shown as formula (I):
（Ⅰ）
wherein: q is the gas permeability, the unit is: ml/Pa/s/m 2 ；
V 1 The unit of the amount of gas of component 1 that permeates through the gas separation membrane (15) is: ml;
P 1 the unit is that the gas pressure at the upper end of the gas separation membrane (15) is: pa;
C 11 the molar concentration of the gas is 1 for the upper end component of the gas separation membrane (15);
P 2 the unit is that the gas pressure at the lower end of the gas separation membrane (15) is: pa;
C 12 the molar concentration of the gas is the lower end component 1 of the gas separation membrane (15);
t is the time spent from the start of the test to the end of the test, and the unit is: s;
s is the cross-sectional area of the gas separation membrane (15);
and (3) calculating a separation coefficient: the formula of the separation coefficient calculation of the component 1 and the component 2 is shown as a formula (II):
（Ⅱ）
Wherein: c (C) 11 The molar concentration of the upper end component 1 of the gas separation membrane;
C 12 the molar concentration of the component 1 at the lower end of the gas separation membrane;
C 21 the molar concentration of the upper end component 2 of the gas separation membrane;
C 22 the molar concentration of the lower end component 2 of the gas separation membrane;
method II, unsteady state method test:
the unsteady state method is a test based on a device formed by a second unsteady state method gas circuit structure in the upper part structure of the gas separation membrane and the optional two structures at the lower part of the gas separation membrane;
the unsteady state method comprises the following testing steps:
step one S11: the gas separation membrane activation pretreatment comprises: installing a gas separation membrane with the area S on a gas separation membrane clamp, and heating the gas separation membrane by an upper cavity and a lower cavity of the gas separation membrane clamp to desorb impurity gas adsorbed on the surface of the gas separation membrane; simultaneously, the second mass flow controller controls the purge gas in the second gas source to flow out at a certain flow rate, the first four-way valve is switched into a state that the first interface is communicated with the fourth interface, the second interface is communicated with the third interface, the first interface is isolated from the second interface, and the third interface is isolated from the fourth interface, and the purge gas flowing out from the second mass flow controller flows out through the upper end of the gas separation membrane; the third mass flow controller controls the purge gas in the third gas source to flow out at a certain flow rate, the third four-way valve is switched into a state that the first interface is communicated with the fourth interface, the second interface is communicated with the third interface, the first interface is isolated from the second interface, and the third interface is isolated from the fourth interface, and the purge gas flowing out from the third mass flow controller flows out through the lower end of the gas separation membrane; the purging gas flowing through the upper end and the lower end of the gas separation membrane blows away the impurity gas desorbed by heating;
Step two S12: a gas permeation and separation process comprising: the gas separation membrane clamp stops heating to enable the gas separation membrane to return to room temperature, the second mass flow controller is closed, the first mass flow controller controls the test gas in the first gas source to flow out at a certain flow rate, the test gas is mixed gas, the concentration of each component is known, the permeation rate and separation coefficient test of two components in the mixed gas are described below, the other components are similar, the names of the two components are component 1 and component 2, and the molar concentration of the component 1 is C 11 Component 2 has a molar concentration of C 21 The method comprises the steps of carrying out a first treatment on the surface of the At this time, the first pressure sensor records that the gas pressure at the upper end of the gas separation membrane is P 1 The method comprises the steps of carrying out a first treatment on the surface of the The third four-way valve is switched into the connection of the first interface and the second interface, the connection of the third interface and the fourth interface, the isolation of the first interface and the fourth interface and the isolation of the second interface and the third interfaceStarting a gas circulation pump to enable gas in a connecting pipeline of a lower cavity of the gas separation membrane clamp, a third four-way valve, the gas circulation pump and the three devices to circulate, wherein a test gas component 1 and a component 2 at the upper end of the gas separation membrane penetrate into the lower end of the gas separation membrane through the gas separation membrane to enable the gas pressure at the lower end of the gas separation membrane to rise, and when the gas pressure at the lower end of the gas separation membrane is not risen and is stabilized to a certain pressure value any more, the second pressure sensor records that the pressure value is P 2 ；
Step S13: detection of permeation and separation gas: the second four-way valve is switched to a state in which the first interface is communicated with the second interface, the third interface is communicated with the fourth interface, the first interface is isolated from the fourth interface, the second interface is isolated from the third interface, the third four-way valve is switched to a state in which the first interface is communicated with the fourth interface, the second interface is communicated with the third interface, the first interface is isolated from the second interface, the third interface is isolated from the fourth interface, the third mass flow controller controls the gas in the third gas source to blow the gas circularly flowing in the step S12 to the interface of the gas detector, and the molar concentration of the component 1 in the gas detected to flow is C 12 Component 2 has a molar concentration of C 22 The gas amount of component 1 permeated from the upper end of the gas separation membrane to the lower end of the gas separation membrane at the time of detection duration t was V 1 The gas amount of component 2 is V 2 ；
Step S14: and (3) calculating the permeability and the separation coefficient:
and (3) calculating the permeability: the permeability is the gas quantity of a certain component gas in the mixed gas at the upper end of the gas separation membrane (15) in unit time, unit pressure difference and unit cross section area of the gas separation membrane (15) entering the lower end of the gas separation membrane (15) in a permeation mode, and the calculation formula is shown in formula (I);
And (3) calculating a separation coefficient: the formula of the separation coefficient calculation of the component 1 and the component 2 is shown as a formula (II).
According to the technical scheme provided by the invention, the tester for the permeability and the separation coefficient of the gas separation membrane and the testing method thereof can adopt two principles of a steady-state method and an unsteady-state method to realize the testing of the permeability and the separation coefficient of the gas separation membrane, and meanwhile, the gas with weak permeability and separation capability is enriched and then is detected, so that the detection sensitivity is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a steady state method architecture of a gas separation membrane permeability and separation coefficient tester;
FIG. 2 is a schematic diagram showing an unsteady state method structure of a gas separation membrane permeability and separation coefficient tester;
fig. 3 and 4 are schematic structural views of the four-way valve in different working states;
In the figure, a first air source, a second air source, a third air source, a first mass flow controller, a second mass flow controller, a third mass flow controller, a back pressure valve, a first four-way valve, a first pressure sensor, a gas separation membrane clamp and a gas separation membrane clamp are arranged in sequence, wherein the first air source, the second air source, the third air source, the first mass flow controller, the second mass flow controller, the third mass flow controller, the back pressure valve, the first four-way valve, the second pressure sensor, the gas separation membrane clamp and the gas separation membrane clamp are arranged in sequence, the device comprises a second pressure sensor, a second four-way valve, a third four-way valve, a fourth pressure sensor, a cold trap pipe and a cold trap cup.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
Unless specifically stated or limited otherwise, the terms "mounted," "connected," and "fixed" are to be construed broadly, and may be, for example, either fixed or removable; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the description of the present invention, it should be noted that the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. Wherein, the terms "first air source 1", "second air source 2" and "third air source 3" are three air sources located at different positions, and the types of the air sources can be the same or different. Wherein the terms "first mass flow controller 4", "second mass flow controller 5" and "third mass flow controller 6" are three mass flow controllers located at different positions and having the same function, and all of the mass flow controllers are used for controlling a certain flow rate of gas. The first four-way valve 8, the second four-way valve 12 and the third four-way valve 16 are three four-way valves which are positioned at different positions and have the same functions, and are provided with four interfaces shown in fig. 2 and 3, namely an interface one 18, an interface two 19, an interface three 20 and an interface four 21; the four-way valve has two communication states, and the first communication state is shown in fig. 3: the first interface 18 is communicated with the fourth interface 21, the second interface 19 is communicated with the third interface 20, the first interface 18 is isolated from the second interface 19, and the third interface 20 is isolated from the fourth interface 21; the second communication state is as shown in fig. 4: the first interface 18 is communicated with the second interface 19, the third interface 20 is communicated with the fourth interface 21, the first interface 18 is isolated from the fourth interface 21, and the second interface 19 is isolated from the third interface 20; the two communication states of the four-way valve can be switched through electrical control.
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
The gas path structure of the gas separation membrane permeability and separation coefficient tester is divided into an upper part and a lower part by taking the gas separation membrane 15 as a boundary, namely, a gas path structure at the upper part of the gas separation membrane 15 and a gas path structure at the lower part of the gas separation membrane 15; the gas path structure at the lower part of the gas separation membrane 15 comprises two optional structures, namely a steady-state method gas path structure and an unsteady-state method gas path structure.
Exemplary device one
As shown in fig. 1, the gas separation membrane permeability and separation coefficient tester is composed of a gas path structure at the upper part of a gas separation membrane 15 and a steady state method gas path structure at the lower part of the gas separation membrane 15, and comprises: the first gas source 1 is used for storing test gas, wherein the test gas can be pure component gas or mixed gas; a second gas source 2 and a third gas source 3 for storing a purge gas; the air inlet of the first mass flow controller 4 is connected with the air outlet of the first air source 1, and the first mass flow controller 4 controls the air in the first air source 1 to flow out at a certain flow rate; the air inlet of the second mass flow controller 5 is connected with the air outlet of the second air source 2, and the second mass flow controller 5 controls the air in the second air source 2 to flow out at a certain flow rate; the air outlets of the first mass flow controller 4 and the second mass flow controller 5 are combined together and connected with an interface I18 of the first four-way valve 8; the gas separation membrane clamp 10 comprises an upper cavity and a lower cavity, the gas separation membrane 15 is clamped between the upper cavity and the lower cavity, both ends of the upper cavity and the lower cavity of the gas separation membrane clamp 10 are respectively provided with a gas inlet and a gas outlet, the gas inlet of the upper cavity is connected with a fourth interface 21 of the first four-way valve 8, and the gas outlet of the upper cavity is connected with a third interface 20 of the first four-way valve 8; the first pressure sensor 9 is used for measuring the pressure at the upper end of the gas separation membrane 15, and is fixedly arranged on a branch of a connecting pipeline of a port IV 21 of the first four-way valve 8 and an air inlet of the upper cavity of the gas separation membrane clamp 10; the second port 19 of the first four-way valve 8 is connected with the first port 18 of the second four-way valve 12, and the second port 19 of the second four-way valve 12 is connected with the tail gas exhaust port; the gas detector interface 13 is used for connecting a gas detector 14, the gas inlet of the gas detector interface is connected with an interface IV 21 of the second four-way valve 12, the gas outlet of the gas detector interface is connected with a tail gas exhaust port, the gas detector 14 only extracts a part of gas analysis flowing through the gas detector interface 13, and the residual gas flows out from the tail gas exhaust port.
A third mass flow controller 6, the air inlet of which is connected with the air outlet of the third air source 3, the third mass flow controller 6 controls the air in the third air source 3 to flow out at a certain flow rate; the air outlet of the third mass flow controller 6 is connected with the air inlet of the lower cavity of the gas separation membrane clamp 10, and the air outlet of the lower cavity of the gas separation membrane clamp 10 is connected with the third port 20 of the second four-way valve 12; the second pressure sensor 11 is used for measuring the pressure at the lower end of the gas separation membrane 15, and is fixedly arranged on a branch of a connecting pipeline of the third mass flow controller 6 and the gas inlet of the lower cavity of the gas separation membrane clamp 10; the third mass flow controller 6 controls the purge gas in the third gas source 3 to blow the test gas permeated from the upper end of the gas separation membrane 15 to the lower end of the gas separation membrane 15 to the gas detector interface 13 to be detected by the gas detector 14.
The optional exemplary apparatus for testing the permeability and separation coefficient of the gas separation membrane further comprises a cold trap tube 22 and a cold trap cup 23, wherein the cold trap tube 22 is installed between the lower cavity of the gas separation membrane fixture 10 and the second four-way valve 12, and the connection manner is as follows: an air inlet of the cold trap pipe 22 is connected with an air outlet of the lower cavity of the gas separation membrane fixture 10, the air outlet of the cold trap pipe 22 is connected with an interface III 20 of the second four-way valve 12, the cold trap pipe 22 is arranged in a cold trap cup 23, and liquid refrigerant is put in the cold trap cup 23; when the concentration of the gas penetrating from the upper end of the gas separation membrane 15 to the lower end of the gas separation membrane 15 is low and cannot be detected by the gas detector 14, the third mass flow controller 6 controls the purge gas to blow the test gas penetrating from the upper end of the gas separation membrane 15 to the lower end into the cold trap tube 22, and as the cold trap tube 22 is immersed in the liquid refrigerant with low temperature, the test gas blown into the cold trap tube 22 is condensed and enriched in the cold trap tube 22 for a certain period of time, the cold trap cup 23 is removed, the temperature of the cold trap tube 22 is instantaneously raised, the liquid or solid test gas condensed in the cold trap tube 22 is gasified, and then the purge gas controlled by the third mass flow controller 6 is blown to the gas detector interface 13 and detected by the gas detector 14.
Exemplary device two
The gas separation membrane permeability and separation coefficient tester shown in fig. 2 may be composed of a gas path structure of an upper portion of the gas separation membrane 15 and a gas path structure of a lower portion of the gas separation membrane 15, including: the first gas source 1 is used for storing test gas, wherein the test gas can be pure component gas or mixed gas; a second gas source 2 and a third gas source 3 for storing a purge gas; the air inlet of the first mass flow controller 4 is connected with the air outlet of the first air source 1, and the first mass flow controller 4 controls the air in the first air source 1 to flow out at a certain flow rate; the air inlet of the second mass flow controller 5 is connected with the air outlet of the second air source 2, and the second mass flow controller 5 controls the air in the second air source 2 to flow out at a certain flow rate; a third mass flow controller 6, the air inlet of which is connected with the air outlet of the third air source 3, the third mass flow controller 6 controls the air in the third air source 3 to flow out at a certain flow rate; the air outlets of the first mass flow controller 4 and the second mass flow controller 5 are combined together and connected with an interface I18 of the first four-way valve 8; the air outlet of the third mass flow controller 6 is connected with a fourth interface 21 of the third four-way valve 16. The gas separation membrane fixture 10 comprises an upper cavity and a lower cavity, the gas separation membrane 15 is clamped between the upper cavity and the lower cavity, two ends of the upper cavity of the gas separation membrane fixture 10 are provided with a gas inlet and a gas outlet, the gas inlet of the upper cavity is connected with a fourth interface 21 of the first four-way valve 8, the gas outlet of the upper cavity is connected with a third interface 20 of the first four-way valve 8, the gas inlet of the lower cavity is connected with a gas outlet of the gas circulation pump 17, and the gas outlet of the lower cavity is connected with a second interface 19 of the third four-way valve 16.
The gas circulation pump 17 is a device for circulating gas, the gas inlet of the gas circulation pump is connected with the first port 18 of the third four-way valve 16, and the gas outlet of the gas circulation pump is connected with the gas inlet of the lower cavity of the gas separation membrane fixture 10; the first pressure sensor 9 is fixedly arranged on a branch of a connecting pipeline of the interface four 21 of the first four-way valve 8 and the upper cavity of the gas separation membrane clamp 10, and can test the gas pressure at the upper end of the gas separation membrane 15; the second pressure sensor 11 is fixedly arranged on a branch of a connecting pipeline of the lower cavity air inlet of the gas separation membrane clamp 10 and the gas circulating pump 17, and can test the gas pressure at the lower end of the gas separation membrane 15.
When the third four-way valve 16 is switched to the communication state shown in fig. 4: the first port 18 is communicated with the second port 19, the third port 20 is communicated with the fourth port 21, the first port 18 is isolated from the fourth port 21, the second port 19 is isolated from the third port 20, and the gas circulation pump 17 is started to enable gas in a closed space formed by the gas circulation pump 17, the lower cavity of the gas separation membrane fixture 10, the third four-way valve 16 and connecting pipelines thereof to circulate. The second port 19 of the first four-way valve 8 is connected with the first port 18 of the second four-way valve 12, the second port 19 of the second four-way valve 12 is connected with the tail gas exhaust port, and the third port 20 of the second four-way valve 12 is connected with the third port 20 of the third four-way valve 16. The gas detector interface 13 is used for connecting with the gas detector 14, the gas inlet of the gas detector interface is connected with the fourth interface 21 of the second four-way valve 12, the gas outlet of the gas detector interface is connected with the tail gas exhaust, the gas detector 14 only extracts a part of gas analysis flowing through the gas detector interface 13, and the residual gas flows out from the tail gas exhaust.
The exemplary device one and exemplary device two also have the following features:
alternatively, both the upper and lower chambers of the gas separation membrane holder 10 have a heating function, and may be heat-treated for the gas separation membrane 15.
Optionally, the gas separation membrane permeability and separation coefficient tester further includes a back pressure valve 7, the back pressure valve 7 is disposed on a connecting pipeline between the first four-way valve 8 and the second four-way valve 12, an air inlet of the back pressure valve 7 is connected with a second port 19 of the first four-way valve 8, and an air outlet of the back pressure valve 7 is connected with a first port 18 of the second four-way valve 12. The back pressure valve 7 can control the front end gas path to be higher than normal pressure, so that the gas pressure at the upper end of the gas separation membrane 15 can be maintained in a high-pressure state, and the permeability and the separation coefficient of the gas separation membrane 15 under different pressure differences can be tested.
Alternatively, the gas detector 14 may be a thermal conductivity detector, a mass spectrum detector, an infrared spectrum detector, or the like.
When the invention works, the permeability and the separation coefficient of the gas separation membrane 15 can be tested, the testing methods are divided into a steady state method and an unsteady state method, and the testing steps of the two testing methods are respectively described below.
Method one, steady state method:
the steady state method, which means that the gas pressure at the upper and lower ends of the gas separation membrane 15 is always stable, and the pressure at the lower end of the gas separation membrane 15 is not increased due to the permeation of the gas at the upper end of the gas separation membrane 15 to the lower end of the gas separation membrane 15, is a test based on the above-described exemplary apparatus one;
the steady state method test steps are as follows:
step one S01: the gas separation membrane 15 activation pretreatment includes: the gas separation membrane 15 having an area S is mounted on the gas separation membrane holder 10, and the upper and lower chambers of the gas separation membrane holder 10 heat the gas separation membrane 15 to desorb impurity gas adsorbed on the surface of the gas separation membrane 15. Meanwhile, the second mass flow controller 5 controls the purge gas in the second gas source 2 to flow out at a certain flow rate, and the first four-way valve 8 is switched to a state that the first port 18 is communicated with the fourth port 21, the second port 19 is communicated with the third port 20, the first port 18 is isolated from the second port 19, the third port 20 is isolated from the fourth port 21, and the purge gas flowing out from the second mass flow controller 5 flows out through the upper end of the gas separation membrane 15; the third mass flow controller 6 controls the purge gas in the third gas source 3 to flow out through the lower end of the gas separation membrane 15 at a certain flow rate; the purge gas flowing through the upper and lower ends of the gas separation membrane 15 blows away the impurity gas desorbed by heating.
Step two S02: gas permeation and separation, comprising: stopping the heating of the gas separation membrane holder 10 allows the gas separation membrane 15 to return to room temperature, the second mass flow controller 5 is closed, andthe first mass flow controller 4 controls the flow of the test gas in the first gas source 1, which is a mixed gas and has known concentrations of the components, through the upper end of the gas separation membrane 15 at a certain flow rate, and the permeation rate and separation coefficient test of two components in the mixed gas are described below, and the other components are similar, so that the two components are named as a component 1 and a component 2, and the molar concentration of the component 1 is C 11 Component 2 has a molar concentration of C 21 The method comprises the steps of carrying out a first treatment on the surface of the At this time, the first pressure sensor 9 records the gas pressure at the upper end of the gas separation membrane 15 as P 1 The method comprises the steps of carrying out a first treatment on the surface of the The test gas component 1 and the component 2 at the upper end of the gas separation membrane 15 permeate through the gas separation membrane 15 to enter the lower end of the gas separation membrane, and the second pressure sensor 11 records that the pressure value at the lower end of the gas separation membrane 15 is P 2 ；
The gas in the first gas source 1 can be a pure component gas; in the case of pure gas, only the permeability was tested.
The optional regulation position is set up in the back pressure valve 7 between the first four-way valve 8 and the second four-way valve 12, make the pressure of the upper end of the gas separation membrane 15 rise, the lower end of the gas separation membrane 15 maintains the normal pressure, thus test the permeability and separation coefficient of the gas separation membrane 15 under certain pressure difference.
Step S03: permeation and separation gas detection: the third mass flow controller 6 controls the gas in the third gas source 3 to blow the gas permeated from the upper end of the gas separation membrane 15 to the lower end of the gas separation membrane 15 to the gas detector interface 13, and the gas detector 14 detects the molar concentration of the component 1 in the flowing gas as C 12 Component 2 has a molar concentration of C 22 The amount of gas of the component 1 permeated from the upper end of the gas separation membrane 15 to the lower end of the gas separation membrane 15 at the time of detection time t is V 1 The gas amount of component 2 is V 2 ；
Step S04: and (3) calculating the permeability and the separation coefficient:
and (3) calculating the permeability: the permeability is the gas quantity of a certain component gas in the mixed gas at the upper end of the gas separation membrane (15) in unit time, unit pressure difference and unit cross section area of the gas separation membrane (15) entering the lower end of the gas separation membrane (15) in a permeation mode, and the calculation formula is shown as formula (I):
（Ⅰ）
wherein: q is the gas permeability, the unit is: ml/Pa/s/m 2 ；
V 1 The unit of the amount of gas of component 1 that permeates through the gas separation membrane (15) is: ml;
P 1 the unit is that the gas pressure at the upper end of the gas separation membrane (15) is: pa;
C 11 the molar concentration of the gas is 1 for the upper end component of the gas separation membrane (15);
P 2 The unit is that the gas pressure at the lower end of the gas separation membrane (15) is: pa;
C 12 the molar concentration of the gas is the lower end component 1 of the gas separation membrane (15);
t is the time spent from the start of the test to the end of the test, and the unit is: s;
s is the cross-sectional area of the gas separation membrane (15);
and (3) calculating a separation coefficient: the formula of the separation coefficient calculation of the component 1 and the component 2 is shown as a formula (II):
（Ⅱ）
wherein: c (C) 11 Is the molar concentration of component 1 at the upper end of the gas separation membrane 15;
C 12 is the molar concentration of the lower end component 1 of the gas separation membrane 15;
C 21 is the molar concentration of the upper end component 2 of the gas separation membrane 15;
C 22 is the molar concentration of the lower end component 2 of the gas separation membrane 15;
method two, unsteady state method:
the unsteady state method is that the gas pressure at the upper end of the gas separation membrane 15 is always stable, and the gas at the upper end of the gas separation membrane 15 permeates to the lower end of the gas separation membrane 15 to raise the pressure at the lower end of the gas separation membrane 15, and the method is based on one test performed by the second exemplary device;
the unsteady state method comprises the following testing steps:
step one S11: the gas separation membrane 15 activation pretreatment includes: the gas separation membrane 15 having an area S is mounted on the gas separation membrane holder 10, and the upper and lower chambers of the gas separation membrane holder 10 heat the gas separation membrane 15 to desorb impurity gas adsorbed on the surface of the gas separation membrane 15. Meanwhile, the second mass flow controller 5 controls the purge gas in the second gas source 2 to flow out at a certain flow rate, and the first four-way valve 8 is switched to a state that the first port 18 is communicated with the fourth port 21, the second port 19 is communicated with the third port 20, the first port 18 is isolated from the second port 19, the third port 20 is isolated from the fourth port 21, and the purge gas flowing out from the second mass flow controller 5 flows out through the upper end of the gas separation membrane 15; the third mass flow controller 6 controls the purge gas in the third gas source 3 to flow out at a certain flow rate, and the third four-way valve 16 is switched to a state that the first port 18 is communicated with the fourth port 21, the second port 19 is communicated with the third port 20, the first port 18 is isolated from the second port 19, the third port 20 is isolated from the fourth port 21, and the purge gas flowing out from the third mass flow controller 6 flows out through the lower end of the gas separation membrane 15; the purge gas flowing through the upper and lower ends of the gas separation membrane 15 blows away the impurity gas desorbed by heating.
Step two S12: gas permeation and separation, comprising: the gas separation membrane fixture 10 stops heating to recover the gas separation membrane 15 to room temperature, the second mass flow controller 5 is closed, the first mass flow controller 4 controls the test gas in the first gas source 1 to flow out at a certain flow rate, the test gas is a mixed gas with known concentration of each component, the permeation rate and separation coefficient test of two components in the mixed gas are described below, and other components are similar, the two components are named as component 1 and component 2, and the molar concentration of the component 1 is C 11 Component 2 has a molar concentration of C 21 ；
At this time, the first pressure sensor 9 records the gas pressure at the upper end of the gas separation membrane 15 as P 1 The method comprises the steps of carrying out a first treatment on the surface of the The third four-way valve 16 is switched to be communicated and connected between the first interface 18 and the second interface 19The third port 20 is communicated with the fourth port 21, the first port 18 is isolated from the fourth port 21, the second port 19 is isolated from the third port 20, the gas circulation pump 17 is started to enable the gas in the connecting pipelines of the lower cavity of the gas separation membrane clamp 10, the third four-way valve 16, the gas circulation pump 17 and the three devices to circulate, at the moment, the test gas component 1 and the component 2 at the upper end of the gas separation membrane 15 penetrate into the lower end of the gas separation membrane 15 through the gas separation membrane 15 to enable the gas pressure at the lower end of the gas separation membrane 15 to rise, and when the gas pressure at the lower end of the gas separation membrane 15 is no longer risen and is stabilized to a certain pressure value, the second pressure sensor 11 records that the pressure value is P 2 ；
The gas in the first gas source 1 can be pure component gas, and if the gas is pure gas, only the permeability is tested;
the optional regulation position is set up in the back pressure valve 7 between the first four-way valve 8 and the second four-way valve 12, make the upper end pressure of the gas separation membrane 15 rise, thus test the adsorption penetration adsorbed under certain pressure difference.
Step S13: detection of permeation and separation gas: the second four-way valve 12 is switched to a communication state in which the first port 18 is communicated with the second port 19, the third port 20 is communicated with the fourth port 21, the first port 18 is isolated from the fourth port 21, the second port 19 is isolated from the third port 20, then the communication state of the third four-way valve 16 is switched to a state in which the first port 18 is communicated with the fourth port 21, the second port 19 is communicated with the third port 20, the first port 18 is isolated from the second port 19, the third port 20 is isolated from the fourth port 21, the third mass flow controller 6 controls the gas in the third gas source 3 to blow the gas circularly flowing in the step S12 to the interface 13 of the gas detector, and the gas detector 14 detects that the molar concentration of the component 1 in the flowing gas is C 12 Component 2 has a molar concentration of C 22 The gas amount of component 1 permeated from the upper end of the gas separation membrane to the lower end of the gas separation membrane at the time of detection duration t was V 1 The gas amount of component 2 is V 2 ；
Step S14: and (3) calculating the permeability and the separation coefficient:
and (3) calculating the permeability: the permeability is the gas quantity of a certain component gas in the mixed gas at the upper end of the gas separation membrane (15) in unit time, unit pressure difference and unit cross section area of the gas separation membrane (15) entering the lower end of the gas separation membrane (15) in a permeation mode, and the calculation formula is shown in formula (I);
and (3) calculating a separation coefficient: the formula of the separation coefficient calculation of the component 1 and the component 2 is shown as a formula (II).
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (10)
1. The gas separation membrane permeability and separation coefficient tester is characterized in that a gas path structure of the tester is divided into an upper part and a lower part by taking a gas separation membrane (15) as a boundary, namely, a gas path structure at the upper part of the gas separation membrane (15) and a gas path structure at the lower part of the gas separation membrane (15); the gas separation membrane (15) upper portion gas circuit structure includes: the air inlet of the first mass flow controller (4) is connected with the air outlet of the first air source (1); an air inlet of the second mass flow controller (5) is connected with an air outlet of the second air source (2); the air outlets of the first mass flow controller (4) and the second mass flow controller (5) are combined together and connected with an interface I (18) of the first four-way valve (8); the gas separation membrane clamp (10) comprises an upper cavity and a lower cavity, a gas separation membrane (15) is clamped between the upper cavity and the lower cavity, both ends of the upper cavity and the lower cavity of the gas separation membrane clamp (10) are respectively provided with a gas inlet and a gas outlet, the gas inlet of the upper cavity is connected with a fourth interface (21) of the first four-way valve (8), and the gas outlet of the upper cavity is connected with a third interface (20) of the first four-way valve (8); the first pressure sensor (9) is fixedly arranged on a branch of a connecting pipeline of a fourth interface (21) of the first four-way valve (8) and an air inlet of the upper cavity of the gas separation membrane clamp (10); the second port (19) of the first four-way valve (8) is connected with the first port (18) of the second four-way valve (12), and the second port (19) of the second four-way valve (12) is connected with the tail gas exhaust port; an air inlet of the gas detector interface (13) is connected with an interface IV (21) of the second four-way valve (12), an air outlet of the gas detector interface (13) is connected with the tail gas exhaust port, and the gas detector (14) is connected to the gas detector interface (13); the gas path structure of the lower part of the gas separation membrane (15) comprises: a steady-state method gas circuit structure or an unsteady-state method gas circuit structure; the steady state method gas circuit structure includes: the air inlet of the third mass flow controller (6) is connected with the air outlet of the third air source (3), the air outlet of the third mass flow controller (6) is connected with the air inlet of the lower cavity of the gas separation membrane clamp (10), the air outlet of the lower cavity of the gas separation membrane clamp (10) is connected with the third port (20) of the second four-way valve (12), and the second pressure sensor (11) is fixedly arranged on a branch of a connecting pipeline of the air outlet of the third mass flow controller (6) and the air inlet of the lower cavity of the gas separation membrane clamp (10); or, the gas path structure at the lower part of the gas separation membrane (15) is the unsteady state method gas path structure, comprising: the air inlet of third mass flow controller (6) is connected with the gas outlet of third air supply (3), and the gas outlet of third mass flow controller (6) is connected with interface four (21) of third cross valve (16), the air inlet of gas separation membrane anchor clamps (10) lower chamber is connected with the gas outlet of gas circulation pump (17), the air outlet of gas separation membrane anchor clamps (10) lower chamber is connected with interface two (19) of third cross valve (16), the air inlet of gas circulation pump (17) is connected with interface one (18) of third cross valve (16), and second pressure sensor (11) are fixed to be set up on the branch way of the connecting line of the air inlet of the lower chamber of gas separation membrane anchor clamps (10) and gas circulation pump (17), interface three (20) of third cross valve (16) with interface three (20) of second cross valve (12) are connected.
2. The gas separation membrane permeability and separation coefficient tester according to claim 1, wherein the upper and lower chambers of the gas separation membrane holder (10) have a heating function for heat-treating the gas separation membrane (15).
3. The gas separation membrane permeability and separation coefficient tester according to claim 1, wherein a back pressure valve (7) can be installed on a connecting pipeline between the first four-way valve (8) and the second four-way valve (12), an air inlet of the back pressure valve (7) is connected with a second interface (19) of the first four-way valve (8), and an air outlet of the back pressure valve (7) is connected with a first interface (18) of the second four-way valve (12).
4. The gas separation membrane permeability and separation coefficient tester according to claim 1, wherein the first four-way valve (8), the second four-way valve (12) and the third four-way valve (16) are three four-way valves with the same function and located at different positions, each four-way valve is provided with four interfaces, namely an interface one (18), an interface two (19), an interface three (20) and an interface four (21), the first four-way valve (8), the second four-way valve (12) and the third four-way valve (16) are provided with two communication states, and the first communication state is: the first interface (18) is communicated with the fourth interface (21), the second interface (19) is communicated with the third interface (20), the first interface (18) is isolated from the second interface (19), and the third interface (20) is isolated from the fourth interface (21); the second communication state is: the first interface (18) is communicated with the second interface (19), the third interface (20) is communicated with the fourth interface (21), the first interface (18) is isolated from the fourth interface (21), and the second interface (19) is isolated from the third interface (20).
5. The gas separation membrane permeability and separation coefficient tester according to claim 1, wherein a cold trap tube (22) is installed between the second four-way valve (12) and a lower cavity of the gas separation membrane clamp (10) in a steady state method gas path structure at the lower part of the gas separation membrane (15), and the connection mode is as follows: an air inlet of the cold trap tube (22) is connected with an air outlet of a lower cavity of the gas separation membrane clamp (10), the air outlet of the cold trap tube (22) is connected with an interface III (20) of the second four-way valve (12), the cold trap tube (22) is arranged in a cold trap cup (23), and liquid refrigerant is put into the cold trap cup (23).
6. The gas separation membrane permeability and separation coefficient tester according to claim 1, wherein the third four-way valve (16) in the unsteady state air passage structure of the lower portion of the gas separation membrane (15) is switched to the following communication state: the first interface (18) is communicated with the second interface (19), the third interface (20) is communicated with the fourth interface (21), the first interface (18) is isolated from the fourth interface (21), the second interface (19) is isolated from the third interface (20), and the gas circulation pump (17) is started to enable gas in a closed space formed by the gas circulation pump (17), the lower cavity of the gas separation membrane clamp (10), the third four-way valve (16) and connecting pipelines of the third four-way valve to circulate.
7. The gas separation membrane permeability and separation factor tester according to claim 1, wherein the gas detector (14) is a thermal conductivity detector or a mass spectrum detector or an infrared spectrum detector.
8. The method for testing the permeability and the separation coefficient of the gas separation membrane based on the tester for the permeability and the separation coefficient of the gas separation membrane according to claims 1 to 6 is characterized in that the permeability and the separation coefficient of the gas separation membrane (15) are tested, and the testing method is divided into a steady-state method and an unsteady-state method, and comprises the following steps:
method one, steady state method:
the steady state method is a test based on a tester consisting of a gas path structure at the upper part of the gas separation membrane (15) and a steady state method gas path structure at the lower part of the gas separation membrane (15);
the steady state method test steps are as follows:
step one S01: a gas separation membrane (15) activation pretreatment comprising: the gas separation membrane (15) with the area S is arranged on a gas separation membrane clamp (10), an upper cavity and a lower cavity of the gas separation membrane clamp (10) heat the gas separation membrane (15) to enable impurity gas adsorbed on the surface of the gas separation membrane (15) to be desorbed, meanwhile, the second mass flow controller (5) controls purge gas in the second gas source (2) to flow out at a certain flow rate, and the first four-way valve (8) is switched into a state that the first interface (18) is communicated with the fourth interface (21), the second interface (19) is communicated with the third interface (20), the first interface (18) is isolated from the second interface (19), the third interface (20) is isolated from the fourth interface (21), and the purge gas flowing out from the second mass flow controller (5) flows out through the upper end of the gas separation membrane (15); the third mass flow controller (6) controls purge gas in the third gas source (3) to flow out through the lower end of the gas separation membrane (15) at a certain flow rate; purge gas flowing through the upper end and the lower end of the gas separation membrane (15) blows away impurity gas desorbed by heating;
Step two S02: gas permeation and separation, comprising: the gas separation membrane clamp (10) stops heating to enable the gas separation membrane (15) to return to room temperature, the second mass flow controller (5) is closed, the first mass flow controller (4) controls the test gas in the first gas source (1) to flow out from the upper end of the gas separation membrane (15) at a certain flow rate, the test gas is mixed gas and the concentration of each component is known, the permeation rate and separation coefficient test of two components in the mixed gas are described below, the two components are named as component 1 and component 2, and the molar concentration of the component 1 is C 11 Component 2 has a molar concentration of C 21 The method comprises the steps of carrying out a first treatment on the surface of the At this time, the first pressure sensor (9) records that the gas pressure at the upper end of the gas separation membrane (15) is P 1 The method comprises the steps of carrying out a first treatment on the surface of the The test gas component 1 and the component 2 at the upper end of the gas separation membrane (15) permeate into the lower end of the gas separation membrane (15) through the gas separation membrane (15), and the second pressure sensor (11) records that the pressure value at the lower end of the gas separation membrane (15) is P 2 ；
Step S03: permeation and separation gas detection: the third mass flow controller (6) controls the gas in the third gas source (3) to permeate from the upper end of the gas separation membrane (15) to the lower end of the gas separation membrane (15) The gas is blown to a gas detector interface (13), and the gas detector (14) detects that the molar concentration of the component 1 in the flowing gas is C 12 Component 2 has a molar concentration of C 22 The gas detector (14) detects the gas amount V of the component 1 penetrating from the upper end of the gas separation membrane (15) to the lower end of the gas separation membrane (15) at the time of t 1 The gas amount of component 2 is V 2 ；
Step S04: and (3) calculating the permeability and the separation coefficient:
and (3) calculating the permeability: the permeability is the gas quantity of a certain component gas in the mixed gas at the upper end of the gas separation membrane (15) in unit time, unit pressure difference and unit cross section area of the gas separation membrane (15) entering the lower end of the gas separation membrane (15) in a permeation mode, and the calculation formula is shown as formula (I):
（Ⅰ）
wherein: q is the gas permeability, the unit is: ml/Pa/s/m 2 ；
V 1 The unit of the amount of gas of component 1 that permeates through the gas separation membrane (15) is: ml;
P 1 the unit is that the gas pressure at the upper end of the gas separation membrane (15) is: pa;
C 11 the molar concentration of the gas is 1 for the upper end component of the gas separation membrane (15);
P 2 the unit is that the gas pressure at the lower end of the gas separation membrane (15) is: pa;
C 12 the molar concentration of the gas is the lower end component 1 of the gas separation membrane (15);
t is the time spent from the start of the test to the end of the test, and the unit is: s;
s is the cross-sectional area of the gas separation membrane (15);
and (3) calculating a separation coefficient: the formula of the separation coefficient calculation of the component 1 and the component 2 is shown as a formula (II):
（Ⅱ）
wherein: c (C) 11 Is the molar concentration of the upper end component 1 of the gas separation membrane (15);
C 12 is the molar concentration of the lower end component 1 of the gas separation membrane (15);
C 21 is the molar concentration of the upper end component 2 of the gas separation membrane (15);
C 22 is the molar concentration of the lower end component 2 of the gas separation membrane (15);
method two, unsteady state method:
the unsteady state method is a test based on a tester consisting of a gas path structure at the upper part of the gas separation membrane (15) and an unsteady state method gas path structure at the lower part of the gas separation membrane (15);
the unsteady state method comprises the following testing steps:
step one S11: a gas separation membrane (15) activation pretreatment comprising: installing a gas separation membrane (15) with the area S on a gas separation membrane clamp (10), and heating the gas separation membrane (15) by an upper cavity and a lower cavity of the gas separation membrane clamp (10) to desorb impurity gas adsorbed on the surface of the gas separation membrane (15); meanwhile, the second mass flow controller (5) controls purge gas in the second gas source (2) to flow out at a certain flow rate, the first four-way valve (8) is switched into a state that the first interface (18) is communicated with the fourth interface (21), the second interface (19) is communicated with the third interface (20), the first interface (18) is isolated from the second interface (19), the third interface (20) is isolated from the fourth interface (21), and the purge gas flowing out from the second mass flow controller (5) flows out through the upper end of the gas separation membrane (15); the third mass flow controller (6) controls purge gas in the third gas source (3) to flow out at a certain flow rate, and the third four-way valve (16) is switched to a state that the first interface (18) is communicated with the fourth interface (21), the second interface (19) is communicated with the third interface (20), the first interface (18) is isolated from the second interface (19), the third interface (20) is isolated from the fourth interface (21), and the purge gas flowing out from the third mass flow controller (6) flows out through the lower end of the gas separation membrane (15); purge gas flowing through the upper end and the lower end of the gas separation membrane (15) blows away impurity gas desorbed by heating;
Step two S12: gas permeation and separation, comprising: the gas separation membrane clamp (10) stops heating to enable the gas separation membrane (15) to return to room temperature, the second mass flow controller (5) is closed, the first mass flow controller (4) controls the test gas in the first gas source (1) to flow out at a certain flow rate, the test gas is mixed gas, the concentration of each component is known, the permeation rate and separation coefficient test of two components in the mixed gas are described below, the two components are named as component 1 and component 2, and the molar concentration of the component 1 is C 11 Component 2 has a molar concentration of C 21 The method comprises the steps of carrying out a first treatment on the surface of the At this time, the first pressure sensor (9) records that the gas pressure at the upper end of the gas separation membrane (15) is P 1 The method comprises the steps of carrying out a first treatment on the surface of the The third four-way valve (16) is switched to be communicated between the first interface (18) and the second interface (19), between the third interface (20) and the fourth interface (21), between the first interface (18) and the fourth interface (21) and between the second interface (19) and the third interface (20), the gas circulation pump (17) is started to enable the gas sealed in the lower cavity of the gas separation membrane clamp (10), the third four-way valve (16), the gas circulation pump (17) and the connecting pipelines of the three devices to circulate, at the moment, the test gas component 1 and the component 2 at the upper end of the gas separation membrane (15) permeate into the lower end of the gas separation membrane (15) through the gas separation membrane (15) to enable the gas pressure at the lower end of the gas separation membrane (15) to rise, and when the gas pressure at the lower end of the gas separation membrane (15) is not risen and is stabilized to a certain pressure value, the second pressure sensor (11) records that the pressure value is P 2 ；
Step S13: detection of permeation and separation gas: the second four-way valve (12) is switched to a communication state in which the first interface (18) is communicated with the second interface (19), the third interface (20) is communicated with the fourth interface (21), the first interface (18) is isolated from the fourth interface (21), the second interface (19) is isolated from the third interface (20), and then the communication state of the third four-way valve (16) is switched to a communication state in which the first interface (18) is communicated with the fourth interface (21), the second interface (19) is communicated with the third interface (20), and the first interface is communicated with the fourth interface(18) In a state of being isolated from the second interface (19), the third interface (20) and the fourth interface (21), the third mass flow controller (6) controls the gas in the third gas source (3) to blow the gas circularly flowing in the step S12 to the interface (13) of the gas detector, and the gas detector (14) detects that the molar concentration of the flowing component 1 is C 12 Component 2 has a molar concentration of C 22 The gas detector (14) permeates the gas separation membrane (15) from the upper end to the lower end of the gas separation membrane (15) when the detection duration is t, and the gas amount of the component 1 is V 1 The gas amount of component 2 is V 2 ；
Step S14: and (3) calculating the permeability and the separation coefficient:
and (3) calculating the permeability: the permeability is the gas quantity of a certain component gas in the mixed gas at the upper end of the gas separation membrane (15) in unit time, unit pressure difference and unit cross section area of the gas separation membrane (15) entering the lower end of the gas separation membrane (15) in a permeation mode, and the calculation formula is shown in formula (I);
And (3) calculating a separation coefficient: the formula of the separation coefficient calculation of the component 1 and the component 2 is shown as a formula (II).
9. The method for testing the permeability and separation coefficient of a gas separation membrane according to claim 8, wherein the gas in the first gas source (1) is either a pure component gas, and only the permeability is tested when the pure component gas is used.
10. The method for testing the permeability and the separation coefficient of the gas separation membrane according to claim 8, wherein the back pressure valve (7) is arranged between the first four-way valve (8) and the second four-way valve (12) at the adjusting position, so that the pressure of the upper end of the gas separation membrane (15) is increased, and the testing of the permeability and the separation coefficient of the gas separation membrane (15) under a certain pressure difference is realized.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002331219A (en) * | 2001-01-25 | 2002-11-19 | Ube Ind Ltd | Apparatus and method for separating and recovering halogen compound gas |
| TW201137338A (en) * | 2010-04-23 | 2011-11-01 | Wei-Hsin Chen | An apparatus and method of precisely measuring permeance of a membrane |
| CN102901699A (en) * | 2012-11-08 | 2013-01-30 | 济南兰光机电技术有限公司 | Device and method for testing gas separation performance of film |
| CN103575630A (en) * | 2013-10-23 | 2014-02-12 | 中国广州分析测试中心 | Measuring method and device for simultaneously measuring membrane permeability of each gas mixed gas |
| DE102013002724B3 (en) * | 2013-02-12 | 2014-07-03 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method and device for determining the permeation rate of barrier materials |
| CN103969165A (en) * | 2014-04-30 | 2014-08-06 | 东北大学 | Device and method for simultaneously testing permeability of compact rocks under transient state and steady state |
| CN108088778A (en) * | 2017-12-06 | 2018-05-29 | 中国科学院武汉岩土力学研究所 | A kind of rock type materials permeability, porosity testing device |
| CN109701365A (en) * | 2018-12-21 | 2019-05-03 | 北京放射性核素实验室 | Atmosphere xenon enrichment hollow fiber film assembly combines and measures the device of its effect |
| CN109883894A (en) * | 2019-03-29 | 2019-06-14 | 西南石油大学 | A kind of superhigh temperature super-pressure stable state air water mutually seeps test device and test method |
| CN217901489U (en) * | 2021-12-06 | 2022-11-25 | 淮阴师范学院 | Bi-component gas separation testing device |
-
2023
- 2023-02-27 CN CN202310169933.2A patent/CN116148155B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002331219A (en) * | 2001-01-25 | 2002-11-19 | Ube Ind Ltd | Apparatus and method for separating and recovering halogen compound gas |
| TW201137338A (en) * | 2010-04-23 | 2011-11-01 | Wei-Hsin Chen | An apparatus and method of precisely measuring permeance of a membrane |
| CN102901699A (en) * | 2012-11-08 | 2013-01-30 | 济南兰光机电技术有限公司 | Device and method for testing gas separation performance of film |
| DE102013002724B3 (en) * | 2013-02-12 | 2014-07-03 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method and device for determining the permeation rate of barrier materials |
| CN103575630A (en) * | 2013-10-23 | 2014-02-12 | 中国广州分析测试中心 | Measuring method and device for simultaneously measuring membrane permeability of each gas mixed gas |
| CN103969165A (en) * | 2014-04-30 | 2014-08-06 | 东北大学 | Device and method for simultaneously testing permeability of compact rocks under transient state and steady state |
| CN108088778A (en) * | 2017-12-06 | 2018-05-29 | 中国科学院武汉岩土力学研究所 | A kind of rock type materials permeability, porosity testing device |
| CN109701365A (en) * | 2018-12-21 | 2019-05-03 | 北京放射性核素实验室 | Atmosphere xenon enrichment hollow fiber film assembly combines and measures the device of its effect |
| CN109883894A (en) * | 2019-03-29 | 2019-06-14 | 西南石油大学 | A kind of superhigh temperature super-pressure stable state air water mutually seeps test device and test method |
| CN217901489U (en) * | 2021-12-06 | 2022-11-25 | 淮阴师范学院 | Bi-component gas separation testing device |
Non-Patent Citations (4)
| Title |
|---|
| 一种非稳态气体渗流条件下岩石渗透特性参数计算方法及应用;刘健;陈亮;王春萍;马利科;王驹;;岩土力学(第05期);全文 * |
| 变压膜渗透空气分离制氧实验研究;杜雄伟;刘应书;;低温与特气(第04期);全文 * |
| 聚砜中空纤维膜去除气流中的CO_2、H_2O和O_2;周崇阳;冯淑娟;周国庆;金玉仁;徐辉;徐景明;梁俊福;;核化学与放射化学(第05期);q我 * |
| 非稳态法气体渗透率测试装置的设计;万军凤;;科技经济导刊(第27期);全文 * |
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