CN106492642A - A kind of low temperature membrane separation device performance test methods - Google Patents
A kind of low temperature membrane separation device performance test methods Download PDFInfo
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- CN106492642A CN106492642A CN201610851276.XA CN201610851276A CN106492642A CN 106492642 A CN106492642 A CN 106492642A CN 201610851276 A CN201610851276 A CN 201610851276A CN 106492642 A CN106492642 A CN 106492642A
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- 239000012528 membrane Substances 0.000 title claims abstract description 81
- 238000000926 separation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 11
- 238000011056 performance test Methods 0.000 title claims abstract description 7
- 238000012360 testing method Methods 0.000 claims abstract description 48
- 230000008595 infiltration Effects 0.000 claims abstract description 47
- 238000001764 infiltration Methods 0.000 claims abstract description 47
- 230000035699 permeability Effects 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000011156 evaluation Methods 0.000 claims abstract description 6
- 238000005259 measurement Methods 0.000 claims abstract description 6
- 230000002631 hypothermal effect Effects 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 155
- 230000008859 change Effects 0.000 claims description 11
- 238000011144 upstream manufacturing Methods 0.000 claims description 9
- 239000000344 soap Substances 0.000 claims description 8
- 239000012466 permeate Substances 0.000 claims description 6
- 230000003139 buffering effect Effects 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000004587 chromatography analysis Methods 0.000 claims 1
- 239000010408 film Substances 0.000 description 29
- 238000005516 engineering process Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 238000011426 transformation method Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000009715 pressure infiltration Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of low temperature membrane separation device performance test methods, membrane separator is placed in thermostat, on the membrane material in the membrane separator, thermal resistance is connected with, at the air inlet of the membrane separator, is provided with pressure gauge I;The vent outlet that oozes of the membrane separator is connected with test branch road I and test branch road II by threeway I, using the infiltration atmospheric pressure in the pressure transducer measurement infiltration gas surge tank, the percentage composition that each component gas in mixed gas infiltration gas is measured using the gas chromatograph, the membrane separator is made to be under different low temperature and room temperature by adjusting the temperature in the thermostat, the selectivity and permeability of under Different hypothermia and room temperature membrane material are tested and calculated respectively, and curve chart is drawn out, complete the evaluation that film properties are varied with temperature.The present invention can test out permeability and selectivity of the membrane separation device in low temperature environment to mixed gas, and complete the evaluation that film properties are varied with temperature.
Description
Technical field
The invention belongs to gas membrane Seperation Technology field, more particularly to a kind of low temperature membrane separation device performance test side
Method.
Background technology
Gas membrane Seperation Technology has started to business application in 20 century 70s, the technology be mainly characterized by energy consumption low,
The clearer production technology of pollution-free, simple to operate, easy maintenance.Critical component in membrane separation device is membrane module, and membrane module is thin,
Good pressure-resistant performance, the surface area required for can ensure that when atm number is processed.Membrane material mostly is polymer, in the case of room temperature,
There is mutually restriction between permeability of the membrane and selectivity.But, under cryogenic, the selectivity of film significantly can increase
Plus, and permeability does not have big change, therefore, reduces temperature, it is possible to increase the performance of film.
It is presently used for determining the infiltrative test device of membrane module much, but these test devices has one altogether
Same deficiency, can only determine a kind of permeability of clean gas every time, or mixed gas permeate the permeability of gas, it is impossible to once same
When determine mixed gas infiltration gas in the thin permeability of the membrane of each component gas permeation.
Gas chromatograph is a kind of modern analysis and test instrument that reproducible, sensitivity is high and separating power is strong, is not required to
The purge gass system of accurate control flow is wanted, appropriate method and chromatographic condition is selected, can rapidly and accurately be measured gaseous mixture
The content of each component gas in body, operation used time are short.
U.S.'s test and the test method ASTM D1434-82 (2009) of materialogy meetingε1" plastic sheeting and thin slice breathability
The standard method of measure " (Standard Method for Determining Gas Permeability
Characteristics of Plastic Film and Sheeting), and China's standard GB/T1038-2000 " plastics
Thin film and thin slice gas-premeable test method " all surveys permeability of the membrane using constant volume pressure differential method.
Content of the invention
The present invention provides a kind of low temperature membrane separation device performance test for solving technical problem present in known technology
Method, can test out permeability and selection of the membrane separation device in low temperature environment to mixed gas using the method
Property, and complete the evaluation that film properties are varied with temperature.
The present invention is adopted the technical scheme that by solving technical problem present in known technology:A kind of low temperature membrance separation
Device performance method of testing, membrane separator is placed in thermostat, is connected with heat on the membrane material in the membrane separator
Resistance, is provided with pressure gauge I at the air inlet of the membrane separator;The membrane separator ooze vent outlet by threeway I with
Test branch road I and test branch road II connect, and the test branch road I includes the ball valve I being sequentially connected, permeates gas surge tank, vacuum
Valve and vacuum pump, are provided with pressure transducer on the infiltration gas surge tank, and the ball valve I is connected with the threeway I;The survey
Examination branch road II includes ball valve II, threeway II and the gas chromatograph being sequentially connected, and in the threeway II is provided with soap film flowmeter,
Pressure gauge II is provided with the pipeline for connecting the ball valve II and the threeway II;When the infiltration for needing to test single clean gas
Property and mixed gas overall permeability when, open described test branch road I, close described test branch road II, using the pressure
Infiltration atmospheric pressure in the sensor measurement infiltration gas surge tank, according to formulaCalculate film
The permeability of material for gaseous, wherein:PAGas permeation rate, cm3(STP)/cm2·s·Pa;In stable transmission
When, the arithmetic mean of instantaneous value of gas pressure change, P in unit interval infiltration gas surge tanka/ s, by pressure transducer record infiltration
The change of the endosmosis ventilative pressure of gas surge tank, after in unit interval endosmosis ventilating buffering tank, gas pressure change is stable, measures many
Group data calculation art meansigma methodss are obtainedV infiltration gas buffering tank volumes, cm3;S membrane areas, cm2;The temperature of T membrane materials
Degree, K are obtained by thermal resistance;P1-P2The pressure reduction of membrane material upstream and downstream both sides, Pa, P1The pressure of film upstream side, by pressure
Table I is obtained, P2The pressure in film downstream, is obtained by pressure transducer;T0, P0Temperature and pressure under standard state, T0=
273.15K,P0=1.0133 × 105Pa;When the respective permeability of each component gas in test mixing gas is needed, institute is closed
Test branch road I is stated, the test branch road II is opened, using each component gas in gas chromatograph measurement mixed gas infiltration gas
The percentage composition of body, according to formulaCalculate permeability of the membrane material to A gases in mixed gas, root
According to formulaMembrane permeability of the membrane material to B gases in mixed gas is calculated, wherein:P′AA gases
Infiltration rate, cm3(STP)/cm2·s·Pa;PB' B gas permeation rates, cm3(STP)/cm2·s·Pa;Q permeates gas
Flow, cm3/ s, is obtained by soap film flowmeter;S membrane areas, cm2;P1Film upstream side pressure, Pa, obtained by pressure gauge I;
P2Film downstream lateral pressure, Pa, obtained by pressure gauge II;XAThe percentage composition of A gases in unstripped gas;XBB gas in unstripped gas
The percentage composition of body;YAIn infiltration gas, the percentage composition of A gases, is measured by gas chromatograph;YBB gases in infiltration gas
Percentage composition, measured by gas chromatograph;According to formulaFilm is calculated to A gases in mixed gas and B gases
Selectivity;Make the membrane separator under different low temperature and room temperature by adjusting the temperature in the thermostat, divide
The selectivity and permeability of membrane material under Different hypothermia and room temperature is not tested and calculated, and draws out curve chart, complete film property
The evaluation that can be varied with temperature.
The present invention has the advantages and positive effects of:
1) present invention has built low temperature membrane separation device, membrane material is separated gas under cryogenic, is film
Separate gas and provide a kind of new thinking.Present research is greatly gathered in the modification to membrane material, improves film
Separating effect, but separate modal polymeric film material for gas, under normal temperature condition, between permeability and selectivity
There is implacable " shifting " equilibrium relation (trade-off).This device carries out membrance separation at low temperature, can make film
Material has simultaneously high permeability and selectivity, improves membrane separating effect, and is verified by test.
2) present invention using gas chromatograph is reproducible, sensitivity is high, separating power is strong and many testing laboratories all
The characteristics of having configuration, simplicity achieve the combination of gas chromatograph and constant volume transformation method, test pure gas using constant volume transformation method
Body and the overall permeability of mixed gas, can once while quick and precisely measuring mixed gas passes through membrane material using gas chromatogram
The component gas permeability of material, can study mixed gas through when various composition infiltration rate is influenced each other.
3) temperature of the present invention by regulating thermostatic device, makes membrane material in different low temperature environments, and then tests out
Permeability of the membrane energy under the conditions of Different hypothermia, draws the infiltration with temperature as abscissa, with permeability or selectivity as vertical coordinate
Performance curve, can intuitively find out film properties variation with temperature under cryogenic.
Description of the drawings
Fig. 1 is the test system structure schematic diagram of the application present invention.
In figure:1st, unstripped gas surge tank, 2, ball valve III, 3, flow controller, 4, pressure gauge I, 5, thermostat, 6, film point
From device, 7, thermal resistance, 8, ball valve IV, 9, moisture recorder, 10, threeway I, 11, ball valve I, 12, infiltration gas surge tank, 13, vacuum
Valve, 14, vacuum pump, 15, pressure transducer, 16, ball valve II, 17, pressure gauge II, 18, soap film flowmeter, 19, threeway II, 20,
Gas chromatograph.
Specific embodiment
For content of the invention, feature and effect of the present invention can be further appreciated that, following examples are hereby enumerated, and coordinates accompanying drawing
Describe in detail as follows:
Fig. 1 is referred to, a kind of low temperature membrane separation device performance test methods are placed in membrane separator 6 in thermostat 5,
Thermal resistance 7 is connected with membrane material in the membrane separator 6, at the air inlet of the membrane separator 6 is provided with pressure gauge I
4.
The vent outlet that oozes of the membrane separator 6 is connected with test branch road I and test branch road II by threeway I 10, described
Test branch road I includes ball valve I 11, infiltration gas surge tank 12, vacuum valve 13 and the vacuum pump 14 being sequentially connected, in the infiltration gas
Surge tank 12 is provided with pressure transducer 15, and the ball valve I 11 is connected with the threeway I 10;Described test branch road II include according to
The ball valve II 16 of secondary connection, threeway II 19 and gas chromatograph 20, are provided with soap film flowmeter 18 in the threeway II 19, even
The pipeline for connecing the ball valve II 16 and the threeway II 19 is provided with pressure gauge II 17.
When the overall permeability for needing to test the permeability of single clean gas and mixed gas, the test is opened
Road I, closes the test branch road II, measures the infiltration air pressure in the infiltration gas surge tank 12 using the pressure transducer 15
Power, according to formulaPermeability of the membrane material to gas is calculated, wherein:PAGas infiltration speed
Rate, cm3(STP)/cm2·s·Pa;In stable transmission, gas pressure change in unit interval infiltration gas surge tank 12
Arithmetic mean of instantaneous value, Pa/ s, the change for recording 12 endosmosis ventilative pressure of infiltration gas surge tank by pressure transducer 15, during unit
After in the interior infiltration gas surge tank 12, gas pressure change is stable, measurement multi-group data asks arithmetic mean of instantaneous value to obtain
12 volume of V infiltration gas surge tank, cm3;S membrane areas, cm2;The temperature of T membrane materials, K are obtained by thermal resistance 7;P1-
P2The pressure reduction of membrane material upstream and downstream both sides, Pa, P1The pressure of film upstream side, is obtained by pressure gauge I 4, P2Film downstream
Pressure, is obtained by pressure transducer 15;T0, P0Temperature and pressure under standard state, T0=273.15K, P0=1.0133 ×
105Pa.
When the respective permeability of each component gas in test mixing gas is needed, the test branch road I is closed, institute is opened
Test branch road II is stated, the percentage composition that each component gas in mixed gas infiltration gas is measured using the gas chromatograph 20, root
According to formulaPermeability of the membrane material to A gases in mixed gas is calculated, according to formulaMembrane permeability of the membrane material to B gases in mixed gas is calculated, wherein:P′AA gases infiltration speed
Rate, cm3(STP)/cm2·s·Pa;P′BB gas permeation rates, cm3(STP)/cm2·s·Pa;Q permeates gas flow,
cm3/ s, is obtained by soap film flowmeter 18;S membrane areas, cm2;P1Film upstream side pressure, Pa, obtained by pressure gauge I 4;
P2Film downstream lateral pressure, Pa, obtained by pressure gauge II 17;XAThe percentage composition of A gases, X in unstripped gasBB in unstripped gas
The percentage composition of gas, can be known by detection before testing;YAThe percentage composition of A gases in infiltration gas, by gas phase color
Spectrometer 20 is measured;YBIn infiltration gas, the percentage composition of B gases, is measured by gas chromatograph 20.
According to formulaCalculate selectivity of the film to A gases and B gases in mixed gas.
Make the membrane separator 6 under different low temperature and room temperature by adjusting the temperature in the thermostat 5, divide
The selectivity and permeability of membrane material under Different hypothermia and room temperature is not tested and calculated, and draws out curve chart, complete film property
The evaluation that can be varied with temperature.The moisture recorder 9 being connected with thermal resistance 7 is used for the temperature of recording film.
Fig. 1 is referred to, Fig. 1 shows that a kind of test system of the application present invention, air inlet are led to through unstripped gas surge tank 1
Ball valve III 2, flow controller 3, pressure gauge I 4 is crossed, is entered from the air inlet of membrane separator 6, gas is passed through in membrane separator 6
Permeability and separation, oozes residual air and successively discharges through oozing residual air outlet and ball valve IV 8;Infiltration gas is selected from vent outlet is oozed through threeway I 10
Selecting property enters test system I or test system II.When needing to test the permeability of single clean gas and the entirety of mixed gas
During permeability, before being tested, ball valve I 11 is opened, close ball valve II 16, by vacuum pump 14,13 pairs ooze by vacuum valve
12 evacuation of ventilating buffering tank, after the completion of evacuation, opens ball valve III 2, and membrane separator 6 starts air inlet, and infiltration gas enters infiltration
Gas surge tank 12, measures the infiltration atmospheric pressure in infiltration gas surge tank 12 using pressure transducer 15.When needing test mixing gas
In body during the respective permeability of each component gas, ball valve I 11 is closed, open ball valve II 16, open ball valve III 2, membrane separator 6 is opened
Beginning air inlet, infiltration gas enter gas chromatograph 20 through ball valve II 16, pressure gauge II 17 and threeway II 19, using gas chromatograph
In 20 measurement mixed gas infiltration gas, the percentage composition of each component gas, measures permeating airflow amount by soap film flowmeter 18.
Although being described to the preferred embodiments of the present invention above in conjunction with accompanying drawing, the invention is not limited in
The specific embodiment that states, above-mentioned specific embodiment be only schematically, be not restricted, this area common
Technical staff in the case of without departing from present inventive concept and scope of the claimed protection, may be used also under the enlightenment of the present invention
To make a lot of forms, these are belonged within protection scope of the present invention.
Claims (1)
1. a kind of low temperature membrane separation device performance test methods, it is characterised in that membrane separator is placed in thermostat, in institute
State and thermal resistance is connected with the membrane material in membrane separator, at the air inlet of the membrane separator be provided with pressure gauge I;
The vent outlet that oozes of the membrane separator is connected with test branch road I and test branch road II by threeway I, the test branch road
I includes the ball valve I being sequentially connected, permeates gas surge tank, vacuum valve and vacuum pump, on the infiltration gas surge tank is provided with pressure
Sensor, the ball valve I are connected with the threeway I;Ball valve II that the test branch road II includes being sequentially connected, threeway II are gentle
Chromatography, is provided with soap film flowmeter in the threeway II, sets on the pipeline for connecting the ball valve II and the threeway II
There is pressure gauge II;
When the overall permeability for needing to test the permeability of single clean gas and mixed gas, the test branch road I is opened,
The test branch road II is closed, the infiltration atmospheric pressure in the infiltration gas surge tank is measured using the pressure transducer, according to
FormulaPermeability of the membrane material to gas is calculated, wherein:PAGas permeation rate, cm3
(STP)/cm2·s·Pa;In stable transmission, in unit interval infiltration gas surge tank, the arithmetic of gas pressure change is put down
Average, Pa/ s, the change for recording the endosmosis ventilative pressure of infiltration gas surge tank by pressure transducer, unit interval are endosmosis ventilative slow
Rush in tank gas pressure change stable after, measurement multi-group data asks arithmetic mean of instantaneous value to obtainV infiltration gas buffering tank volumes,
cm3;S membrane areas, cm2;The temperature of T membrane materials, K are obtained by thermal resistance;P1-P2The pressure of membrane material upstream and downstream both sides
Difference, Pa, P1The pressure of film upstream side, is obtained by pressure gauge I, P2The pressure in film downstream, is obtained by pressure transducer;T0,
P0Temperature and pressure under standard state, T0=273.15K, P0=1.0133 × 105Pa;
When the respective permeability of each component gas in test mixing gas is needed, the test branch road I is closed, the survey is opened
Examination branch road II, the percentage composition for measuring each component gas in mixed gas infiltration gas using the gas chromatograph, according to formulaPermeability of the membrane material to A gases in mixed gas is calculated, according to formulaMembrane permeability of the membrane material to B gases in mixed gas is calculated, wherein:PA' A gases infiltration speed
Rate, cm3(STP)/cm2·s·Pa;PB' B gas permeation rates, cm3(STP)/cm2·s·Pa;Q permeates gas flow,
cm3/ s, is obtained by soap film flowmeter;S membrane areas, cm2;P1Film upstream side pressure, Pa, obtained by pressure gauge I;P2Film
Downstream lateral pressure, Pa, obtained by pressure gauge II;XAThe percentage composition of A gases in unstripped gas;XBThe hundred of B gases in unstripped gas
Divide content;YAIn infiltration gas, the percentage composition of A gases, is measured by gas chromatograph;YBThe percentage of B gases in infiltration gas
Content, is measured by gas chromatograph;
According to formulaCalculate selectivity of the film to A gases and B gases in mixed gas;
Make the membrane separator under different low temperature and room temperature by adjusting the temperature in the thermostat, test respectively
The selectivity and permeability of membrane material under Different hypothermia and room temperature is calculated, and draws out curve chart, film properties are completed with temperature
The evaluation of degree change.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110618076A (en) * | 2019-09-19 | 2019-12-27 | 东华大学 | Double-cylinder axial moving bulging type fabric air-lock and air-filtration performance measuring device and method |
CN110618074A (en) * | 2019-09-19 | 2019-12-27 | 东华大学 | Pneumatic fluctuation type double-chamber fabric bulging and air-tightness synchronous measurement device and method |
CN110618077A (en) * | 2019-09-19 | 2019-12-27 | 东华大学 | Device and method for measuring dynamic air filtering and isolating efficiency of fabric and application |
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CN102527245A (en) * | 2010-12-23 | 2012-07-04 | 新奥科技发展有限公司 | Device, system and method for testing separation performance of membrane |
CN202387360U (en) * | 2011-11-07 | 2012-08-22 | 上海奕材环保科技有限公司 | Device for removing moisture in compressed air based on membrane separation technology |
CN203030197U (en) * | 2012-12-12 | 2013-07-03 | 山东恒业石油新技术应用有限公司 | Detection device for performance parameter of single nitrogen separating membrane tube |
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2016
- 2016-09-26 CN CN201610851276.XA patent/CN106492642A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102527245A (en) * | 2010-12-23 | 2012-07-04 | 新奥科技发展有限公司 | Device, system and method for testing separation performance of membrane |
CN202387360U (en) * | 2011-11-07 | 2012-08-22 | 上海奕材环保科技有限公司 | Device for removing moisture in compressed air based on membrane separation technology |
CN203030197U (en) * | 2012-12-12 | 2013-07-03 | 山东恒业石油新技术应用有限公司 | Detection device for performance parameter of single nitrogen separating membrane tube |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110618076A (en) * | 2019-09-19 | 2019-12-27 | 东华大学 | Double-cylinder axial moving bulging type fabric air-lock and air-filtration performance measuring device and method |
CN110618074A (en) * | 2019-09-19 | 2019-12-27 | 东华大学 | Pneumatic fluctuation type double-chamber fabric bulging and air-tightness synchronous measurement device and method |
CN110618077A (en) * | 2019-09-19 | 2019-12-27 | 东华大学 | Device and method for measuring dynamic air filtering and isolating efficiency of fabric and application |
CN110618077B (en) * | 2019-09-19 | 2021-12-10 | 东华大学 | Device and method for measuring dynamic air filtering and isolating efficiency of fabric and application |
CN110618074B (en) * | 2019-09-19 | 2022-07-15 | 东华大学 | Pneumatic wave type double-chamber fabric bulging and air-tightness synchronous measurement device and method |
CN110618076B (en) * | 2019-09-19 | 2022-07-15 | 东华大学 | Double-cylinder axial moving bulging type fabric air-lock and air-filtration performance measuring device and method |
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