CN1830524A - Method of improving gas separation film penetration instrument - Google Patents
Method of improving gas separation film penetration instrument Download PDFInfo
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- CN1830524A CN1830524A CNA2005102007928A CN200510200792A CN1830524A CN 1830524 A CN1830524 A CN 1830524A CN A2005102007928 A CNA2005102007928 A CN A2005102007928A CN 200510200792 A CN200510200792 A CN 200510200792A CN 1830524 A CN1830524 A CN 1830524A
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Abstract
A method for improving the osmosis apparatus with gas separating membrane features that when a constant-pressure volume-varying method is used to measure the gas osmosis of membrane, a vacuumizing method is used at up-stream of membrane pool for exhausting the gas from pipeline and membrane and a capillary soap membrane flowmeter isolated from air is used at the down-stream for measuring the osmotic speed of gas, so effectively preventing the reverse diffusion of gas.
Description
Technical field
The invention belongs to technical field of chemical engineering, relate to a kind of improved new gas diffusion barrier permeameter.
Background technology
Membrane separation technique has efficiently, and advantages such as the energy are saved in environmental protection, have obtained the progress of advancing by leaps and bounds in recent decades, now have been widely used in numerous areas such as food, biology, chemical industry, the energy, environmental protection.Gas separation membrane is the important component part of membrane science and technology, is considered to have most the third generation gas separation of development prospect.The accurate mensuration of the permeability parameter of gas separation membrane (as permeation flux, selectivity etc.) is for the research and development of the improvement of film production process and perfect, new membrane product with use most important.
At present, the method for testing for the permeability parameter of gas separation membrane mainly adopts constant volume transformation force method and constant pressure variable volume method.Constant volume transformation force method is had relatively high expectations to the air-tightness of permeameter gas piping, makes instrument involve great expense; In addition in the mensuration process in order to make the membrane cisterna downstream reach certain condition of high vacuum degree, often need the long pumpdown time, thereby Many researchers adopts cheap, constant pressure variable volume method easily.
Yet, measure in the device of film gas permeability in constant pressure variable volume method, membrane cisterna downstream (low-pressure side) often is connected with atmosphere (soap film flowmeter detection) or sweep gas (chromatogram detection), can make air or chromatogram sweep gas influence the accuracy of measurement result to the upstream (high-pressure side) of film from the downstream back-diffusion of film like this; This method often purges to get rid of residual gas with gas to be measured in the upstream in change measuring the gas process for a long time in addition, has so not only lost time but also wastes the gas of mensuration.Though such flow path device can guarantee normally carrying out of test job, but two problems that exist have influenced the accuracy of measurement result to a certain extent: the one, and the gas that when changing mensuration gas, is difficult to get rid of tunicle adsorbed (inoranic membrane) or dissolves (organic film), the 2nd, the air in membrane cisterna downstream (perhaps chromatogram sweep gas) meeting back-diffusion is to the membrane cisterna upstream.
Summary of the invention
The purpose of this invention is to provide improving one's methods of a kind of gas separation film penetration instrument, be to measure in the gas permeability process of film 1 in constant pressure variable volume method) utilize in the method that the membrane cisterna upstream and downstream vacuumizes and in time get rid of the gas that adsorbs (inoranic membrane) or dissolving (organic film) in gas piping and the film; 2) infiltration rate of using the capillary flowmeter that completely cuts off with air to measure infiltration gas in the membrane cisterna downstream effectively prevents the method for air back-diffusion.Originally improving one's methods to have solved influences two problems that constant pressure variable volume method is measured membrane permeability energy accuracy, can accurately measure the gas permeability parameter of film, and measures the transit time of two kinds of gases before and after saving.
The technical scheme of improving one's methods of film gas permeameter provided by the present invention comprises:
(1) membrane sample to be measured polymer film or inoranic membrane as flat board, tubulose or doughnut is fixed in the membrane cisterna with fluid sealant, is placed in the temperature control box; Gas to be measured is penetrated into the downstream from the upstream of film under the pressure differential effect of film upstream and downstream both sides, and the flux of measuring infiltration gas by capillary flowmeter just can calculate infiltration rate and selectivity.
(2) in the mensuration process, the membrane cisterna upstream uses the pressure maintaining valve controlled pressure more than atmospheric pressure, to avoid because of the not high influence that causes measurement result of gas piping tightness; Mensuration at the flux of downstream infiltration gas adopts capillary soap film flowmeter or other capillary type flow measuring instrument or the controller that completely cuts off, is equipped with mercury, dimethyl silicone polymer or distilled water indicator solution with air, to prevent the air back-diffusion.
(3) measuring a kind of gas or gaseous mixture, when changing the middle transition of surveying another kind of gas or gaseous mixture, adopting upstream and downstream to vacuumize simultaneously, in time removing the residual gas in the gas piping on the one hand at film; Can remove in the film on the other hand and adsorb or dissolved gases; Pumpdown time is 20min～2h, and vacuum is 10
-1～10
-3KPa;
Effect of the present invention and benefit are:
Adopt such scheme, can guarantee the accuracy of the gas permeability parameter measured, save time, laborsaving, easy operating.
Description of drawings
Fig. 1 is a device schematic flow sheet of the present invention.
Among the figure: 1 measures gas, 2 pressure maintaining valves, 3 flow stabilizing valves, 4 vacuum meters, 5 vacuum meter switch valves, 6 Pressure gauges, 7,15 triple valves, 8 vacuumize pump valve, 9 vavuum pumps, 10 gas buffer jars, 11 membrane cisternas, 12 capillary flowmeters or chromatogram, 13,14 emptying, 16 insulating boxs.
Fig. 2 is the structural representation of tabular membrane cisterna.
Among the figure: 17 membrane cisterna loam cakes, 18 membrane cisterna lower covers, 19 aluminium approach adhesive tape, 20 flat sheet membrane, 21 filter paper, 22 porous backing plates, 23 seal washers.
Fig. 3 is the structural representation of tubulose membrane cisterna.
Among the figure: 24 membrane cisterna loam cakes, 25 film hold-down supports, 26 membrane cisterna lower covers, 27 seal washers, 28 tubular films.
The specific embodiment
Be described in detail most preferred embodiment of the present invention below in conjunction with technical scheme and accompanying drawing.
The specific embodiment 1
In Fig. 2, the top and bottom of tabular film 20 are bonded at respectively on the thin adhesive tape 19 of aluminium of annular, pad one deck filter paper and be fixed on the intermediate recess place of membrane cisterna lower cover 18 with glue on porous backing plate 22 is put O shape seal washer 23 well, membrane cisterna loam cake 17 and membrane cisterna lower cover 18 usefulness hex screws fixing on.
In Fig. 1, the membrane cisterna among Fig. 2 is received gas circuit 11 positions that have temperature control box, set the temperature of temperature control box 16.Air intake valve 1, triple valve 7 and 15 are closed, open valve 8, valve 15 turns to and vacuumizes, and at first gets rid of the air in the system of downstream for preventing film fragmentation (inoranic membrane, as carbon membrane etc.) and distortion (polymer film etc.).After treating that downstream vacuum increases to some extent, shut off valve 2 and 13 is opened valve 5, and valve 7 turns to and vacuumizes, and at this moment the upstream and downstream of whole gas circuit is all vacuumizing, and passes through the vacuum of vacuum meter 4 observing systems.After gas clean-up residual in the system totally, shut off valve 15 after the first shut off valve 11, shut off valve 8 again.Feed next gas to be measured, slowly open valve 2, the value of observation vacuum meter 4, after treating that upstream vacuum reaches zero, 15 valves are turned to vacuumize, the downstream begins to charge into gas to be measured, the vacuum for the treatment of upstream and downstream all reaches zero back shut off valve 5, triple valve 7 steering pressure tables.Slowly regulate pressure maintaining valve 2 and flow stabilizing valve 3, observe Pressure gauge 6 and reach required piezometry value, open triple valve 12, detect the infiltration gas flux by flowmeter or chromatogram., measure like this 3～5 times less than 5% up to the error of former and later two values of measuring, get the formula (1) below its mean value substitution, be the infiltration rate of this gas.The infiltration rate of the same other gas of step measurements is the ideal selectivity of this film to these two kinds of gases with the ratio of the infiltration rate of two kinds of pure gas.
Here Q is the infiltration rate of pure gas, and this gas of Flux is by the flux of film, the pressure differential of effective infiltrating area ， Mei film both sides of A film, the thickness of l film.
The specific embodiment 2
In Fig. 3, the two ends of tubular film 28 are sealed with glue, wherein an end is fixed on the bearing 25 with glue, fills up O grommet type seal circle 27 respectively on two sides, the bearing left and right sides, membrane cisterna lower cover 26 precession membrane cisterna loam cakes 24 and fix.
In Fig. 1, with the position that the membrane cisterna among Fig. 3 is received the gas circuit 11 that has insulating box, after the temperature of control insulating box 16.Air intake valve 1, triple valve 7 and 15 are closed, open valve 8, valve 15 turns to and vacuumizes, for preventing that film is broken and being out of shape the air of at first getting rid of in the system of downstream.After treating that downstream pressure will get off, shut off valve 2 and 13 is opened valve 5 and valve 7 is turned to and vacuumizes, and vacuumizes in the upstream and downstream of whole gas circuit, and judges that by vacuum meter 4 vacuum reaches poised state.Shut off valve 15 after elder generation's shut off valve 11, shut off valve 8 again.Feed gas to be measured, slowly open valve 2, the value of observation vacuum meter 4, treat that upstream vacuum reaches zero after, 15 valves are turned to vacuumize, the downstream begins to charge into gas to be measured, the vacuum for the treatment of upstream and downstream all reaches zero back shut off valve 5, triple valve 7 steering pressure tables.Regulate pressure maintaining valve 2 and flow stabilizing valve 3, after observation Pressure gauge 6 reaches the required force value in upstream, open the changing value that triple valve 12 detected in the infiltration gas volume unit times., measure like this 3～5 times less than 5% up to the error of former and later two values of measuring, get the formula (1) below its mean value substitution, be the infiltration rate of this gas.The infiltration rate of the same other gas of step measurements is the ideal selectivity of this film to these two kinds of gases with the ratio of the infiltration rate of two kinds of gases.
Here Q is the infiltration rate of pure gas, and this gas of Flux is by the flux of film, the pressure differential of effective infiltrating area ， Mei film both sides of A film, the thickness of l film.
Embodiment 1
With epoxy glue is thickness 20 Jing, and effectively infiltrating area is 4.15cm
2Circular Kapton be fixed in the membrane cisterna, adopt the specific embodiment 1, obtained this organic film to hydrogen (H
2): 2.2Barrer (1Barrer=10
-10Cm
3(STP) cm cm
-2Zui
-1Lu mHg
-1), carbon dioxide (CO
2): 1.1Barrer, oxygen (O
2): 0.18Barrer, nitrogen (N
2): 0.034Barrer; Selectivity is: H
2/ N
2=64.7, CO
2/ N
2=32.4, O
2/ N
2=5.3.
Embodiment 2
The Kapton charing has been obtained polyimide-based carbon membrane, and its thickness is 15 Jing.This film is fixed in the membrane cisterna with epoxy glue, adopts the specific embodiment 2, obtain this inoranic membrane hydrogen (H
2): 218.6Barrer (1Barrer=10
-10Cm
3(STP) cm cm
-2Zui
-1Lu mHg
-1), carbon dioxide (CO
2): 163.9Barrer, oxygen (O
2): 36.6Barrer, nitrogen (N
2) 3.3Barrer; Selectivity is: H
2/ N
2=66.2, CO
2/ N
2=50.2, O
2/ N
2=11.1.
Embodiment 3
The compound carbon membrane of homemade poly furfuryl alcohol parent tube shape is fixed in the membrane cisterna with epoxy glue, adopts the specific embodiment 2, and adopt gas-chromatography to measure the composition of the mixed gas of film both sides respectively.When feed pressure is 0.1MPa, the mixture of feed body is air (it consists of oxygen 21%, and nitrogen is 79%), and mist consists of oxygen 68% after by film, nitrogen 32%, thus this film is (68/32)/(21/79)=8.0 to the oxygen nitrogen selectivity of air.
Claims (8)
1. a gas separation film penetration instrument improves one's methods, be to measure in the gas permeability process of film in constant pressure variable volume method, utilize upstream and downstream to vacuumize simultaneously, and by measuring the infiltration rate of infiltration gas with the isolated capillary flowmeter of air, it is characterized in that: (1) is fixed on membrane sample to be measured in the membrane cisterna with fluid sealant, is placed in the temperature control box; Gas to be measured is penetrated into the downstream from the upstream of film under the pressure differential effect of film upstream and downstream both sides, measures the fluxmeter of infiltration gas by capillary flowmeter and calculates infiltration rate and selectivity;
(2) measuring a kind of gas, when another kind gas transition to be measured, vacuumizing simultaneously, in time removing the residual gas in the gas piping in the upstream and downstream of film; And remove absorption or be dissolved in gas in the film.
2. according to the improving one's methods of the described a kind of gas separation film penetration instrument of claim 1, it is characterized in that in the mensuration process of film, the membrane cisterna upstream with the pressure maintaining valve controlled pressure more than atmospheric pressure; Adopt the infiltration rate of the capillary flowmeter measurement downstream infiltration gas of secluding air.
3. according to the improving one's methods of the described a kind of gas separation film penetration instrument of claim 1, it is characterized in that the isolated capillary flowmeter of downstream and air is inner soap film flowmeter or other capillary type flow measuring instrument or the controller that indicator solution is housed.
4. according to the improving one's methods of the described a kind of gas separation film penetration instrument of claim 1, it is characterized in that the membrane cisterna upstream and downstream vacuumizes simultaneously in the vacuum, the pumpdown time is 20min～2h, and vacuum is 10-1～10-3Kpa.
5. according to the improving one's methods of the described a kind of gas separation film penetration instrument of claim 1, it is characterized in that the membrane sample that can measure comprises: dull and stereotyped, tubulose or doughnut polymer film or inoranic membrane.
6. according to the improving one's methods of the described a kind of gas separation film penetration instrument of claim 1, it is characterized in that gas to be measured is pure gas or admixture of gas.
7. according to the improving one's methods of the described a kind of gas separation film penetration instrument of claim 3, it is characterized in that the indicator solution of dress in the capillary flowmeter is mercury, dimethyl silicone polymer or distilled water.
8. according to the improving one's methods of the described a kind of gas separation film penetration instrument of claim 6, when it is characterized in that gas to be measured is admixture of gas, with its composition of gas Chromatographic Determination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005102007928A CN100398182C (en) | 2005-12-13 | 2005-12-13 | Method of improving gas separation film penetration instrument |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005102007928A CN100398182C (en) | 2005-12-13 | 2005-12-13 | Method of improving gas separation film penetration instrument |
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| Publication Number | Publication Date |
|---|---|
| CN1830524A true CN1830524A (en) | 2006-09-13 |
| CN100398182C CN100398182C (en) | 2008-07-02 |
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ID=36993120
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101949814A (en) * | 2010-07-30 | 2011-01-19 | 北京科技大学 | Method for measuring methane permeability of marsh gas storage membrane |
| CN111266015A (en) * | 2020-03-05 | 2020-06-12 | 天津工业大学 | Constant volume variable pressure method test system of gas transmittance |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11585794B1 (en) * | 2022-03-29 | 2023-02-21 | United Arab Emirates University | Method and system for gas identification by simultaneous permeation through parallel membranes |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5226932A (en) * | 1991-10-07 | 1993-07-13 | Praxair Technology, Inc. | Enhanced meambrane gas separations |
| US5730780A (en) * | 1993-10-15 | 1998-03-24 | Opus Services, Inc. | Method for capturing nitrogen from air using gas separation membrane |
| KR100534013B1 (en) * | 2003-09-04 | 2005-12-07 | 한국화학연구원 | Titania composite membrane for water/alcohol separation, and Preparation thereof |
| CN100408531C (en) * | 2004-11-22 | 2008-08-06 | 上海蓝景膜技术工程有限公司 | Process for producing high concentration tert-butyl alcohol by permeation vaporization method and products therefrom |
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2005
- 2005-12-13 CN CNB2005102007928A patent/CN100398182C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101949814A (en) * | 2010-07-30 | 2011-01-19 | 北京科技大学 | Method for measuring methane permeability of marsh gas storage membrane |
| CN111266015A (en) * | 2020-03-05 | 2020-06-12 | 天津工业大学 | Constant volume variable pressure method test system of gas transmittance |
| CN111266015B (en) * | 2020-03-05 | 2022-07-08 | 天津工业大学 | Constant volume variable pressure method test system of gas transmittance |
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| CN100398182C (en) | 2008-07-02 |
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Granted publication date: 20080702 Termination date: 20191213 |