CN111266015A - Constant volume variable pressure method test system of gas transmittance - Google Patents
Constant volume variable pressure method test system of gas transmittance Download PDFInfo
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- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
- B01D65/102—Detection of leaks in membranes
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Abstract
The invention discloses a constant volume variable pressure method test system for gas transmittance, which comprises a computer, a data acquisition module, a vacuum pump, a gas cylinder, a pressure transmitter, an upstream gas storage tank, a downstream gas storage tank, a membrane pool assembly and a pressure sensor, wherein the inlets of the upstream gas storage tank and the downstream gas storage tank are respectively provided with the pressure sensor, a pipeline between the upstream gas storage tank and the downstream gas storage tank is sequentially provided with an upstream vacuum-pumping valve, a tee joint and a downstream vacuum-pumping valve, the third end of the tee joint is connected with the vacuum pump, the membrane pool assembly is connected in parallel to the pipeline between the upstream gas storage tank and the downstream gas storage tank, the pressure transmitter, the pressure sensor and a temperature control box are respectively connected with the data acquisition module, and the data acquisition module. The invention reduces the number of valves, has simple and convenient operation, greatly reduces the air leakage rate and the error of a test system, adopts organic glass and aluminum profiles as frames, reduces the weight and the volume of equipment and reduces the cost.
Description
Technical Field
The invention relates to the technical field of gas permeameters, in particular to a constant volume variable pressure method test system for gas transmittance.
Background
The gas separation has huge market and prospect in the fields of energy conservation and emission reduction, green chemical industry, natural gas, biogas purification, hydrogen energy and biological medical treatment. The membrane material transmittance testing system is a testing system for researching intrinsic transmittance and selectivity of materials such as polymers to gas, and is an indispensable characterization means for developing polymer gas separation membrane materials. The gas separation membrane material transmissivity test equipment on the current market is high in gas leakage rate, low in test precision, complex in pipeline, heavy in equipment and incapable of testing high and low temperature and high and low pressure simultaneously. The accuracy of the result obtained by general tests is low, and the application of the membrane separation technology is greatly limited by the defect detection.
The study of the selectivity and permeability of gas separation membrane materials to gases is an important matter for characterizing intrinsic gas separation membrane materials. The judgment of the selectivity and the separation performance of the membrane on gas is the key for researching the gas separation membrane material and is also the precondition of the application of the membrane material. Among the testing methods for gas separation membrane materials, William Koros group of the George Ard in 1986 reported a system for testing gas permeation based on the constant volume variable pressure method [ J.Membr.Sci.1986,29,229-238 ], but the system had complicated valve piping; domestic patents related to gas permeation instruments, such as patents with publication numbers CN209264513 and CN105466831, however, none of the above patents can realize setting of high pressure and high and low temperatures, and no consideration is given to high pressure data, especially data with pressure of 20-30 atm or more, and the actual gas separation is often carried out with pressure of 20-30 atm or even 60 atm or more, and the high pressure condition puts higher requirements on the gas leakage rate of the instrument. In addition, many gas separation occasions are carried out at room temperature or below, and no report is found on an instrument which can test the same set of device at subzero to high temperature and high pressure.
Disclosure of Invention
The invention aims to provide a constant volume variable pressure method testing system for gas permeability, which aims to solve the problems in the prior art, reduce the air leakage rate of equipment and improve the testing precision and range.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a constant volume variable pressure method test system of gas transmittance, which comprises a computer, a data acquisition module, a vacuum pump, a gas cylinder, a pressure transmitter, an upstream gas storage tank, a downstream gas storage tank, a pressure sensor and a membrane pool assembly arranged in a temperature control box, wherein the gas cylinder, the pressure transmitter, the upstream gas storage tank and the downstream gas storage tank are sequentially connected through a stainless steel pipeline, the pressure sensor is arranged at the inlet of each of the upstream gas storage tank and the downstream gas storage tank, an upstream vacuum-pumping valve, a tee joint and a downstream vacuum-pumping valve are sequentially arranged on the pipeline between the upstream gas storage tank and the downstream gas storage tank, the third end of the tee joint is connected with the vacuum pump, the membrane pool assembly is connected in parallel on the pipeline between the upstream gas storage tank and the downstream gas storage tank, and the pressure transmitter, the pressure sensor and the temperature control box are respectively connected with the data acquisition module, the data acquisition module and the vacuum pump are respectively electrically connected with the computer.
Preferably, the membrane pool subassembly includes piece, stainless steel filter screen, membrane and membrane pool lower plate on the membrane pool, the membrane pool upper plate with the corresponding same depressed part that is provided with in membrane pool lower plate center, stainless steel filter screen joint in the depressed part, the membrane is laid on the stainless steel filter screen, the membrane pool upper plate with the membrane pool lower plate be provided with respectively with the through-hole of depressed part intercommunication, the membrane pool upper plate with the membrane pool lower plate is through a plurality of bolted connection.
Preferably, two layers of sealing rings are arranged between the contact surfaces of the upper piece and the lower piece of the membrane pool at intervals, and the sealing rings are positioned on the outer sides of the concave parts.
Preferably, the membrane is an organic membrane material, an inorganic flat membrane material or an organic flat membrane material, and the area of the membrane is 0.1-7cm2The thickness is 1 mu m-20 mm.
Preferably, a total air inlet valve is arranged between the pressure transmitter and the upstream air storage tank, and a detection air inlet valve is arranged between the upstream air storage tank and the membrane pool assembly.
Preferably, the total air inlet valve, the detection air inlet valve, the upstream vacuum-pumping valve, the tee joint, the downstream vacuum-pumping valve and the pipeline are all made of stainless steel.
Preferably, the pressure measured by the first pressure sensor at the outlet of the upstream air storage tank is in the range of 0-800psi, and the test accuracy of the second pressure sensor at the inlet of the downstream air storage tank is 3.5 x 10-4About 1torr, a measuring range of 10-2500torr, a measured pressure change range of 0-1000torr, and an overall gas leakage rate of 10 in the constant volume variable pressure method testing system for gas permeability-8～10-6torr/s。
Preferably, the gas in the gas cylinder is single gas of helium, hydrogen, oxygen, nitrogen, methane, carbon dioxide, hydrogen sulfide, sulfur dioxide or sulfur hexafluoride.
Preferably, the temperature control box panel is made of one or more of aluminum profiles, organic glass, polysulfone plates, polystyrene plates, tetrafluoro plates, metal plates, aluminum plates, phenolic plates, polystyrene plates or wood plates, and the panels are connected through angle steel or aluminum profile connecting pieces.
Preferably, the temperature control range of the temperature control box is-80-100 ℃.
Compared with the prior art, the invention has the following technical effects:
the invention reduces the number of valves, has simple and convenient operation, greatly reduces the air leakage rate and the error of a test system, adopts organic glass and aluminum profiles as frames, reduces the weight and the volume of equipment and reduces the cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic diagram of the structural principle of a constant volume variable pressure method testing system for gas transmittance according to the present invention;
FIG. 2 is a first schematic structural diagram of a membrane cell module in a constant volume pressure swing method testing system for gas permeability according to the present invention;
FIG. 3 is a schematic structural diagram of a membrane cell module in the constant volume pressure swing method testing system for gas permeability according to the present invention;
wherein: the method comprises the following steps of 1-a gas cylinder, 2-a pressure transmitter, 3-a total air inlet valve, 4-a first pressure sensor, 5-an upstream air storage tank, 6-a tee joint, 7-an upstream vacuum-pumping valve, 8-a downstream vacuum-pumping valve, 9-a vacuum pump, 10-a downstream air storage tank, 11-a second pressure sensor, 12-a temperature control box, 13-a computer, 14-a detection air inlet valve, 15-a membrane pool component, 16-an upper membrane pool piece, 17-a sealing ring, 18-a stainless steel filter screen, 19-a membrane, 20-a lower membrane pool piece and 21-a bolt.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
The invention aims to provide a constant volume variable pressure method testing system for gas permeability, which aims to solve the problems in the prior art, reduce the air leakage rate of equipment and improve the testing precision and range.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
As shown in fig. 1to 3: the embodiment provides a constant volume variable pressure method test system of gas transmissivity, including computer 13, data acquisition module, vacuum pump 9, gas cylinder 1, pressure transmitter 2, upstream gas holder 5, low reaches gas holder 10, pressure sensor and set up the membrane pond subassembly 15 in accuse temperature case 12, gas cylinder 1, pressure transmitter 2, upstream gas holder 5 and low reaches gas holder 10 connect gradually through stainless steel pipeline, the gas in the gas cylinder 1 is the single gas in helium, hydrogen, oxygen, nitrogen gas, methane, carbon dioxide, hydrogen sulfide, sulfur dioxide or sulfur hexafluoride. The inlet of the upstream gas storage tank 5 and the inlet of the downstream gas storage tank 10 are both provided with a pressure sensor, the pipeline between the upstream gas storage tank 5 and the downstream gas storage tank 10 is sequentially provided with an upstream vacuum-pumping valve 7, a tee joint 6 and a downstream vacuum-pumping valve 8, the third end of the tee joint 6 is connected with a vacuum pump 9, a membrane pool assembly 15 is connected in parallel with the pipeline between the upstream gas storage tank 5 and the downstream gas storage tank 10, a pressure transmitter 2, the pressure sensor and a temperature control box 12 are respectively connected with a data acquisition module, and the data acquisition module and the vacuum pump 9 are respectively electrically connected with a computer 13.
Specifically, the membrane pool assembly 15 comprises a membrane pool upper piece 16, a stainless steel filter screen 18, a membrane 19 and a membrane pool lower piece 20, the centers of the membrane pool upper piece 16 and the membrane pool lower piece 20 are correspondingly provided with the same concave parts, the stainless steel filter screen 18 is clamped in the concave parts, the membrane is laid on the stainless steel filter screen 18, the membrane 19 is an organic membrane material, an inorganic flat membrane material or an organic flat membrane material, and the area of the membrane is 0.1-7cm2The thickness is 1 mu m-20 mm. The membrane pool upper plate 16 and the membrane pool lower plate 20 are respectively provided with through holes communicated with the concave parts, and the membrane pool upper plate 16 and the membrane pool lower plate 20 are connected through a plurality of bolts 21. Two layers of sealing rings 17 are arranged between the contact surfaces of the membrane pool upper piece 16 and the membrane pool lower piece 20 at intervals, and the sealing rings 17 are positioned on the outer sides of the concave parts.
A total air inlet valve 3 is arranged between the pressure transmitter 2 and the upstream air storage tank 5, and a detection air inlet valve 14 is arranged between the upstream air storage tank 5 and the membrane pool assembly 15. The total air inlet valve 3, the detection air inlet valve 14, the upstream vacuumizing valve 7, the tee joint 6, the downstream vacuumizing valve 8 and the pipeline are all made of stainless steel materials. The gas inlet of the gas bottle 1 is provided with a national standard or European standard card sleeve port quick connection for quickly switching the type of the test gas; the upstream inlet valve comprises a ball valve, needle valve or bellows valve ported by a national or European standard clamp for controlling the inlet of the upstream pressure tank and maintaining the upstream pressure. The tee joint 6 adopts national standard or European standard cutting sleeves, VCR face joint, welding and other connecting modes and is used for reducing the gas leakage rate at the upstream valve.
The pressure sensors comprise a first pressure sensor 4 and a second pressure sensor 11, the pressure measured by the first pressure sensor 4 on the outlet of the upstream air storage tank 5 is 0-800psi, and the test accuracy of the second pressure sensor 11 on the inlet of the downstream air storage tank 11 is 3.5 x 10-4About 1torr, the measured pressure variation range is 0-1000torr, and the integral air leakage rate of the constant volume variable pressure method test system of the gas permeability is 10-8～10-6torr/s. Wherein the upstream of the pipeline is high pressure, and the downstream is low pressure, 1psi ═ 51.7 torr.
The panel of the temperature control box 12 is made of one or more of aluminum profiles, organic glass, polysulfone plates, polystyrene plates, polytetrafluoroethylene plates, metal plates, aluminum plates, phenolic plates, polystyrene plates or wood plates, the thickness of the panel is 5-10 mm, and the panels are connected through angle steel or aluminum profile connecting pieces. The whole instrument of the embodiment is a portable instrument, because the whole instrument uses aluminum profiles and organic glass plates with light weight, the total weight is 20-30 kg except for the pump. A heating device is arranged in the temperature control box 12, and the temperature control range is-80 ℃ to 100 ℃.
The testing method of the gas separation membrane material transmittance testing device comprises the following steps:
and measuring the effective membrane area of the membrane, packaging the membrane to be tested in a stainless steel filter screen of the membrane pool assembly 15, vacuumizing the upstream and the downstream of the test system by a vacuum pump 9, simultaneously discharging gas in a pipeline of the test system, closing all valves and ensuring the vacuum in the test system. And then filling a test gas into the test system: the total air inlet valve 3 on the air bottle 1 is opened, the air storage tank 5at the upstream of the test system is filled with air with proper pressure, and then the total air inlet valve 3 is closed. Gas permeability testing was performed: the gas permeability is calculated by opening the detection intake valve 14, recording the upstream pressure and recording the time-dependent change of the test pressure of the downstream second pressure sensor 11.
Based on the testing principle of the Time-leg method, the intrinsic gas transmittance P (unit Barrer) of the separation membrane material is detected under the condition that the volume of gas in a downstream pipeline is not changed. The gas permeability P and the ideal separation performance a are obtained by testing the change of the downstream pressure of different membranes under a certain gas pressure along with the time.
Where dp/dt is the slope (torr/s), V, obtained during the testdIs the sum of the gas volumes in the piping from the membrane tank assembly 15 and the downstream vacuum valve 8 to the downstream gas holder 5, L is the thickness of the membrane, P isupIs the reading of the first pressure sensor 4, T is the absolute temperature, R is the ideal gas constant, a is the area of the membrane.
The selectivity of the membrane material can be obtained after obtaining the P of the membrane material:
αA/B＝PA/PB；
wherein, PAIs the permeability of gas A, PBThe transmittance of gas B.
Case 1: testing of gas selectivity and permeability data (35 ℃, 2atm) for Polysulfone (PS) membrane materials
A Polysulfone (PS) membrane was put into a stainless steel filter mesh of the membrane cell module 15, the measured pressure of the first pressure sensor 4 was 2atm, the transmittance of the gas was obtained by measuring the change of the pressure of the second pressure sensor 11 with time, and then the separation performance of oxygen/nitrogen was obtained, and table 1 below is an experimental parameter of the separation properties of various gases.
TABLE 1 Experimental parameters for the separation Properties of various gases of polysulfone membranes
Case 2: testing of PI (6FDA-FFDA) Membrane Material gas Selectivity and Permeability data (35 ℃, 2atm)
The PI (6FDA-FFDA) membrane was placed in a stainless steel filter net of the membrane cell assembly 15, and the oxygen/nitrogen separation performance thereof was tested by continuously pressurizing, and the measured pressure of the first pressure sensor 4 was 2 atmospheres, and table 2 below is an experimental parameter of the separation properties of various gases.
Table 2 experimental parameters of the separation properties of various gases of PI membranes
Case 3: testing of Polycarbonate (PC) film Material gas Selectivity and Permeability data (35 ℃, 2atm)
A Polycarbonate (PC) membrane was placed in a stainless steel filter mesh of the membrane cell assembly 15, and the oxygen/nitrogen separation performance thereof was tested by continuously pressurizing, the measurement pressure of the first pressure sensor 4 was 2 atmospheres, and table 3 below is an experimental parameter of the separation properties of various gases.
Table 3 experimental parameters of the separation properties of various gases of PC membranes
Case 4: testing of Silicone rubber Membrane Material gas selectivity and permeability data (35 ℃, 2atm)
A silicon rubber (PDMS) membrane was placed in a stainless steel filter of the membrane cell module 15, and the oxygen/nitrogen separation performance was tested by continuously pressurizing, the measurement pressure of the first pressure sensor 4 was 2 atmospheres, and table 4 below is an experimental parameter of the separation properties of various gases.
Table 4 experimental parameters of separation properties of various gases of PDMS membranes
Case 5: testing high pressure data (pressure 2-15atm)
A polymer membrane was placed in the stainless steel filter mesh of the membrane cell assembly 15 and tested for its oxygen/nitrogen separation performance by continuously pressurizing, the first pressure sensor 4 measured 2 atmospheres, 5 atmospheres to 15 atmospheres, and table 5 below is an experimental parameter for its oxygen/nitrogen separation properties.
TABLE 5 Experimental parameters for oxygen/nitrogen separation Properties at different pressures
Case 6: the high and low temperature performance of the gas permeation of the membrane material is tested, and the temperature is 60 ℃, 40 ℃, 20 ℃, 0 ℃, minus 10 ℃, minus 20 ℃ and minus 30 ℃.
The polymer membrane material was placed in the stainless steel filter screen of the membrane cell assembly 15 of the permeameter, degassed for 2 days, and then tested for gas permeation properties at different temperatures. The permeability of hydrogen, nitrogen and oxygen is mainly tested at different temperatures, and the temperature changes from high temperature to low temperature and from 60 ℃ to-30 ℃. From high temperature to low temperature, the permeability coefficient of the membrane material is gradually reduced, and the selectivity is gradually increased. See table 6 below:
TABLE 6 high and Low temperature Performance of gas permeation of Membrane Material
The principle and the implementation mode of the present invention are explained by applying specific examples in the present specification, and the above descriptions of the examples are only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A constant volume variable pressure method test system of gas transmission rate which characterized in that: comprises a computer, a data acquisition module, a vacuum pump, a gas cylinder, a pressure transmitter, an upstream gas storage tank, a downstream gas storage tank, a pressure sensor and a membrane pool component arranged in a temperature control box, the gas cylinder, the pressure transmitter, the upstream gas storage tank and the downstream gas storage tank are connected in sequence through stainless steel pipelines, the inlets of the upstream air storage tank and the downstream air storage tank are both provided with the pressure sensor, an upstream vacuum-pumping valve, a tee joint and a downstream vacuum-pumping valve are sequentially arranged on a pipeline between the upstream air storage tank and the downstream air storage tank, the third end of the tee joint is connected with the vacuum pump, the membrane pool assembly is connected on the pipeline between the upstream gas storage tank and the downstream gas storage tank in parallel, the pressure transmitter, the pressure sensor and the temperature control box are respectively connected with the data acquisition module, and the data acquisition module and the vacuum pump are respectively electrically connected with the computer.
2. The gas transmission constant volume variable pressure test system according to claim 1, wherein: the membrane pool subassembly includes piece, stainless steel filter screen, membrane and membrane pool lower plate on the membrane pool, the membrane pool upper plate with the corresponding same depressed part that is provided with in membrane pool lower plate center, stainless steel filter screen joint in the depressed part, the membrane is laid in on the stainless steel filter screen, the membrane pool upper plate with the membrane pool lower plate be provided with respectively with the through-hole of depressed part intercommunication, the membrane pool upper plate with the membrane pool lower plate is through a plurality of bolted connection.
3. The gas transmission constant volume variable pressure test system according to claim 2, wherein: two layers of sealing rings are arranged between contact surfaces of the upper piece and the lower piece of the membrane pool at intervals, and the sealing rings are located on the outer sides of the concave parts.
4. The gas transmission constant volume variable pressure test system according to claim 2, wherein: the membrane is an organic flat membrane material or an inorganic flat membrane material, and the area of the membrane is 0.1-7cm2The thickness is 1 mu m-20 mm.
5. The gas transmission constant volume variable pressure test system according to claim 1, wherein: and a total air inlet valve is arranged between the pressure transmitter and the upstream air storage tank, and a detection air inlet valve is arranged between the upstream air storage tank and the membrane pool assembly.
6. The gas transmission constant volume variable pressure test system according to claim 5, wherein: the total air inlet valve, the detection air inlet valve, the upstream vacuumizing valve, the tee joint, the downstream vacuumizing valve and the pipeline are all made of stainless steel materials.
7. The gas transmission constant volume variable pressure test system according to claim 1, wherein: the measuring pressure range of the first pressure sensor on the outlet of the upstream air storage tank is 0-800psi, and the measuring accuracy of the second pressure sensor on the inlet of the downstream air storage tank is 3.5 x 10-4About 1torr, the measured pressure change range is 0-1000torr, and the integral air leakage rate of the constant volume variable pressure method test system of the gas transmittance is 10-8～10-6torr/s。
8. The gas transmission constant volume variable pressure test system according to claim 1, wherein: the gas in the gas cylinder is single gas of helium, hydrogen, oxygen, nitrogen, methane, carbon dioxide, hydrogen sulfide, sulfur dioxide or sulfur hexafluoride.
9. The gas transmission constant volume variable pressure test system according to claim 1, wherein: the material of accuse temperature case panel is one or more in aluminium alloy, organic glass, polysulfone board, polystyrene board, tetrafluoro board, metal sheet, aluminum plate, phenolic aldehyde board, polyphenyl board or plank, connect through angle steel or aluminium alloy connecting piece between the panel.
10. The gas transmission constant volume variable pressure test system according to claim 1, wherein: the temperature control range of the temperature control box is-80-100 ℃.
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