CN114062219A - Breathable film performance test integrated device and operation method thereof - Google Patents

Breathable film performance test integrated device and operation method thereof Download PDF

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Publication number
CN114062219A
CN114062219A CN202111177185.XA CN202111177185A CN114062219A CN 114062219 A CN114062219 A CN 114062219A CN 202111177185 A CN202111177185 A CN 202111177185A CN 114062219 A CN114062219 A CN 114062219A
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pressure
test
gas
module
membrane
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CN114062219B (en
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王建明
陈顺权
郑海荣
宋宏臣
姬婧
郭秋兰
张红斌
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Guangzhou Institute Of Advanced Technology
Shenzhen National Research Institute of High Performance Medical Devices Co Ltd
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Guangzhou Institute Of Advanced Technology
Shenzhen National Research Institute of High Performance Medical Devices Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/082Investigating permeability by forcing a fluid through a sample
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D65/00Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/10Testing of membranes or membrane apparatus; Detecting or repairing leaks
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L5/00Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes
    • G01L5/14Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes for measuring the force of explosions; for measuring the energy of projectiles
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01MTESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00Investigating fluid-tightness of structures
    • G01M3/02Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/26Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N2015/086Investigating permeability, pore-volume, or surface area of porous materials of films, membranes or pellicules

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  • General Physics & Mathematics (AREA)
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  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dispersion Chemistry (AREA)
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  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention relates to the technical field of separation membrane testing, and provides a breathable film performance testing integrated device and an operation method thereof, wherein the device comprises the following steps: the subassembly test module, with the pressure drive control module of subassembly test module tube coupling, with the gas flow detection module that the subassembly test module is connected, respectively with the control system that subassembly test module, pressure drive control module and gas flow detection module communication are connected, the subassembly test module includes: the upper unit is connected with the pressure driving module through a pipeline; the middle unit is provided with a through hole and a non-through hole from bottom to top, the bottom end of the through hole can be detachably connected with a quick screwing joint, the bottom end of the quick screwing joint can be detachably connected with a membrane assembly, and the bottom end of the non-through hole can be detachably connected with a supporting rod. By the technical scheme, comprehensive evaluation and quantitative evaluation on the bursting pressure, the air permeability coefficient and the integrity of the membrane can be realized in the same device, and the testing accuracy and the testing efficiency are higher.

Description

Breathable film performance test integrated device and operation method thereof
Technical Field
The invention relates to the technical field of separation membrane testing, in particular to a breathable film performance testing integrated device and a breathable film performance testing integrated device operation method.
Background
The permeable membrane is taken as an important branch in the field of separation membranes, and has wide application in the fields of food, medicine, biology, environmental protection, chemical industry, water treatment and the like. The performance of the separation membrane is the core for determining the use of the separation membrane, and key parameters of the performance of the existing gas-permeable membrane mainly comprise a gas permeability coefficient, a separation coefficient, mechanical strength, integrity and the like. At present, water permeation detection equipment is generally adopted to detect the integrity of the microporous breathable film, and for the detection of the gas permeability of the breathable film, the gas permeability and the separation coefficient of the separation film cannot be efficiently and accurately tested due to the relatively simple test equipment; in addition, for the test of mechanical strength, especially internal and external burst pressure, the inner side is generally pressurized by water to force the membrane to break, and the burst pressure is monitored.
In the related art, CN103063523A discloses a device and a method for testing the burst resistance pressure and the compressive resistance pressure of a hollow fiber membrane filament, wherein the burst resistance pressure is determined by recording the pressure change in the whole testing process, but the testing accuracy is low, and only the burst resistance pressure and the compressive resistance pressure are tested in a single way, so that it is difficult to realize quantitative testing of multiple performances such as the gas permeability of a gas separation membrane; CN102798586A discloses a novel test system for testing ventilation capacity of a micro-breathable film, utilizes a liquid level meter of a lift tube, adopts isobaric liquid to fill the original space after gas permeation, measures and calculates the rate of gas passing through the micro-breathable film under a certain pressure difference by recording the liquid inlet speed, and has the disadvantages of complicated test, poor accuracy and difficulty in realizing quantitative test of multiple performances such as burst pressure, integrity and the like of the breathable film.
Therefore, a new breathable film performance testing device needs to be researched to solve the problems of lack of a current breathable film performance evaluation method, single equipment testing index, low integration level and the like.
Disclosure of Invention
In view of the above, a need exists for providing an integrated device and an operation method for testing the performance of a breathable membrane, which can implement not only a rapid and accurate test of the burst pressure in the membrane, but also a comprehensive evaluation of the permeability coefficient and integrity of the membrane, and can implement a quantitative evaluation of multiple performances of the breathable separation membrane, and also have high test accuracy and high test efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
an integrated device for testing performance of a breathable film comprises: the subassembly test module, with the pressure drive control module of the top tube coupling of subassembly test module, with the gas flow detection module that the bottom of subassembly test module is connected, respectively with the subassembly test module the pressure drive control module and the control system that the gas flow detection module communication is connected, the subassembly test module includes:
the upper unit, the middle unit and the lower unit are sequentially connected in a sealing manner from top to bottom, and the upper unit is connected with the pressure driving module through a pipeline; the middle unit is provided with a through hole and a non-through hole from bottom to top, the bottom end of the through hole is detachably connected with a quick-screwing joint, the bottom end of the quick-screwing joint is detachably connected with a membrane assembly, and the bottom end of the non-through hole is detachably connected with a support rod.
Preferably, the upper unit includes: an upper cylinder body; the air inlet is arranged on the top surface of the upper cylinder body and is connected with the pressure driving module through a pipeline; a first exhaust port arranged on the side surface of the upper cylinder body, and an exhaust pipeline connected with the first exhaust port is provided with a first electromagnetic valve; and the air inlet side pressure sensor is connected to the side surface of the upper barrel, the height of the connecting position of the air inlet side pressure sensor on the upper barrel is higher than that of the first exhaust port, and the air inlet side pressure sensor is in communication connection with the control system.
Preferably, the lower unit includes: a lower cylinder body; the second exhaust port is arranged on the side face of the lower cylinder body and is connected with the gas flow detection module through a pipeline, and a second electromagnetic valve is arranged on an exhaust pipeline connected with the second exhaust port; and the gas permeation side pressure sensor is connected to the side surface of the lower cylinder body, the height of the connection position of the gas permeation side pressure sensor on the lower cylinder body is higher than that of the second exhaust port, and the gas permeation side pressure sensor is in communication connection with the control system.
Preferably, the upper unit, the middle unit and the lower unit are hermetically connected through threads and sealing rings, and the upper end and the lower end of the middle unit are respectively sleeved in the upper unit and the lower unit;
the middle unit is provided with two through holes and two non-through holes which are distributed in a crossed manner, the through holes and the non-through holes are arranged in a cross manner, the through holes and the quick-screwing joints are arranged in a one-to-one manner, and the non-through holes and the connecting rods are arranged in a one-to-one manner.
Preferably, the support rod is a telescopic adjustable support rod, and the length adjustment range of the telescopic adjustable support rod is 5cm-15 cm; the gas flow detection module is a high-precision gas flowmeter, and the measuring range of the high-precision gas flowmeter is 0-100 ml/min.
Preferably, the pressure driving control module includes: the device comprises a plurality of high-pressure gas cylinders which are arranged in parallel and are respectively connected with the component testing module through pipelines, a pressure reducing valve is respectively arranged on a gas outlet connecting pipeline of each high-pressure gas cylinder, and an electrical proportion regulating valve is arranged on a connecting pipeline close to the component testing module.
An operation method of the integrated device for testing the performance of the breathable film comprises the following steps:
installing two ends of the membrane assembly on quick-screwing connectors of a middle unit of the assembly testing module, adjusting the height of the supporting rod, and straightening the separation membrane downwards to enable the separation membrane to be uniformly distributed;
the middle unit is screwed and hermetically connected with the upper unit and the lower unit, and the component testing module is sequentially connected with the pressure driving and controlling module, the air inlet side pressure sensor, the air outlet side pressure sensor and the air outlet pipeline;
starting a control system, and after the control system normally operates, starting a specified high-pressure gas cylinder and a pressure reducing valve thereof, and adjusting the test pressure;
in a constant pressure mode, setting a pre-detection pressure, a boosting time and a voltage stabilizing time, opening a first electromagnetic valve connected with the upper unit of the component testing module and a second electromagnetic valve connected with the lower unit of the component testing module, controlling boosting, fully discharging air in the device, and then closing the first electromagnetic valve;
after the pressure is stabilized, monitoring the permeation side pressure through a gas permeation side pressure sensor, and if the monitored permeation side pressure is maintained in a specified pressure range for a specified time, determining that the membrane assembly is intact and the air tightness of the device has no problem;
after the pressure of the control device is relieved, carrying out an air permeability coefficient test or a membrane assembly integrity test or an implosion pressure test or carrying out the air permeability coefficient test and the membrane assembly integrity test in sequence or carrying out the air permeability coefficient test and the implosion pressure test in sequence or carrying out the air permeability coefficient test, the membrane assembly integrity test and the implosion pressure test in sequence;
and after the test is finished, controlling and storing data, resetting pressure, dismounting the assembly and turning off a power supply.
Preferably, the permeability coefficient test comprises the steps of:
under a constant pressure mode, setting test pressure, boosting time and voltage stabilization test time, and controlling to start boosting, wherein the value range of the test pressure is 0.1-0.3 MPa, the value range of the boosting time is 5-10 min, and the voltage stabilization test time is not less than 30 min;
when the pressure is constant, detecting the flow of the permeating gas in real time through a gas flow detection module;
calculating the permeability coefficient according to the flow of the permeating gas and a preset formula, wherein the preset formula is as follows:
F=Q/(ΔP·S),
wherein F is characterized by an air permeability coefficient (mL cm)-2·min-1·bar-1) Q is characterized by the permeate gas flow (ml/min) and Δ P is characterized by the transmembrane pressure difference (bar), i.e. the set test pressure; s is characterized by the effective area of the membrane (cm)2)。
Preferably, the membrane module integrity test comprises the steps of:
under a constant pressure mode, setting test pressure, boosting time and pressure stabilization test time, and controlling a nitrogen high-pressure gas cylinder to start boosting, wherein the value range of the test pressure is 0.1-0.3 MPa, the value range of the boosting time is 5-10 min, and the pressure stabilization test time is not less than 30 min;
when the pressure is constant, detecting the flow of the gas penetrating through the nitrogen in real time through a gas flow detection module;
after the pressure of the control device is relieved, an oxygen high-pressure gas cylinder is controlled to start boosting in the same constant pressure mode, and after the pressure is constant, the flow of the gas penetrating through the oxygen is detected in real time through a gas flow detection module;
after the pressure of the control device is relieved, a carbon dioxide high-pressure gas cylinder is controlled to start boosting in the same constant pressure mode, and after the pressure is constant, the flow of the carbon dioxide gas passing through is detected in real time by a gas flow detection module;
calculating the ratio of any two of the flow of the gas penetrating through the nitrogen, the flow of the gas penetrating through the oxygen and the flow of the gas penetrating through the carbon dioxide, wherein the ratio is determined by a larger value and a smaller value;
if any ratio is far larger than 1, the integrity of the membrane component is determined to be good;
if there is a ratio approaching 1, then it is determined that there is a problem with the integrity of the membrane module.
Preferably, the implosion pressure test comprises the steps of:
in the boosting mode, the maximum test pressure and the boosting time are set, and the starting and boosting are controlled;
in the boosting process, the flow of the permeated gas is detected in real time through a gas flow detection module, the test pressure is detected in real time through a pressure sensor at the gas inlet side, and a relation curve graph of the test pressure and the flow of the permeated gas is generated;
if the increase value of the flow rate of the permeating gas in unit time is larger than the preset value, the rupture of the membrane is determined, the pressure rise is stopped, and the maximum value of the test pressure corresponding to the flow rate of the permeating gas in unit time is determined as the bursting pressure in the membrane.
The invention has the beneficial effects that:
(1) the integrated device for testing the performance of the breathable film, provided by the invention, can quickly and accurately test the burst pressure in the film, and meanwhile, can comprehensively evaluate the breathable performance and integrity of the film, so that the real one-machine multi-purpose effect is realized.
(2) The integrated device for testing the performance of the breathable film, provided by the invention, has the advantages of simple structure, convenience in use, suitability for relevant performance tests of PMP (polypropylene) films, PP (polypropylene) separation films, PVDF (polyvinylidene fluoride) hydrophobic films and the like, simple test method, easiness in operation, stable and reliable test structure and high reproducibility.
(3) The integrated device for testing the performance of the breathable film, provided by the invention, is provided with the control system which is in communication connection with each module, has a real-time online numerical value monitoring function, is timely in data feedback and is high in measurement accuracy.
(4) The integrated device for testing the performance of the breathable film is provided with the assembly testing module, the assembly testing module comprises the upper unit, the middle unit and the lower unit which are sequentially and hermetically connected from top to bottom, the film assembly is detachably connected to the middle unit, the film assembly is convenient to detach and replace, and meanwhile, the middle unit is provided with the supporting rod, so that the film assembly is fixed, film threads on the film assembly are straightened as much as possible, the film threads are uniformly distributed, the measurement accuracy is ensured, and the quantitative comparison is facilitated.
(5) The operation method of the breathable film performance test integrated device provided by the invention realizes the ventilation coefficient test, the membrane component integrity test and the implosion pressure test, realizes the quantification of the performance test and is more convenient for comprehensively evaluating the membrane performance.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic structural diagram of an integrated device for testing the performance of a breathable film according to an embodiment of the invention;
FIG. 2 is a schematic top view showing a middle unit of a component testing module in an integrated apparatus for testing the performance of a breathable film according to an embodiment of the invention;
FIG. 3 is a schematic structural diagram of a membrane module installation position after the membrane module is installed in the module test module of the integrated device for testing the breathable film performance according to the embodiment of the invention;
figure 4 shows a schematic structural view of a membrane module according to an embodiment of the invention,
wherein, the corresponding relationship between the reference numbers and the components in fig. 1 to fig. 4 is:
the device comprises a 10 component testing module, an upper unit 102, an upper cylinder 1022, a 1024 air inlet, a 1026 first exhaust port, a 1028 first electromagnetic valve, a 1030 air inlet side pressure sensor, a 104 middle unit, an 1042 through hole, a 1044 non-through hole, a 1046 quick-screwing joint, a 1048 support rod, a 106 lower unit, a 1062 lower cylinder, a 1064 second exhaust port, a 1066 second electromagnetic valve, a 1068 gas permeation side pressure sensor, a 108 sealing ring, a 20 pressure driving and controlling module, a 202 high-pressure gas cylinder, a 204 pressure reducing valve, a 206 electrical proportional regulating valve, a 30 gas flow monitoring module, a 40 control system, a 50 membrane component and 502 membrane wires.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be further clearly and completely described below with reference to the embodiments of the present invention. It should be noted that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1 to 4, an integrated apparatus for testing the performance of a breathable film according to an embodiment of the present invention includes: the device comprises a pressure driving control module 20, an assembly testing module 10, a gas flow detection module and a control system 40, wherein the top of the assembly testing module 10 is connected with a pressure driving module through a pipeline, the bottom of the assembly testing module 10 is connected with the gas flow detection module through a pipeline, and the control system 40 is respectively in communication connection with the assembly testing module 10, the pressure driving module and the gas flow detection module. The component test module 10 includes: the upper unit 102, the middle unit 104 and the lower unit 106 are sequentially and hermetically connected from top to bottom, the upper unit 102 is connected with the pressure driving module through a pipeline, the middle unit 104 is provided with a through hole 1042 and a non-through hole 1044 from bottom to top, the bottom end of the through hole 1042 is detachably connected with the quick-screwing connector 1046, the bottom end of the quick-screwing connector 1046 is detachably connected with the membrane component 50, and the bottom end of the non-through hole 1044 is detachably connected with the supporting rod 1048. The membrane module 50 is installed below the middle unit 104 through the quick-screwing connector 1046, the membrane wires 502 on the membrane module 50 are straightened through the support rod 1048 to be evenly arranged and convenient to test, the structure of the membrane module 50 is as shown in fig. 4, the membrane wires 502 are sealed by PU pipes with the diameter of 10mm or 8mm through epoxy glue, then end faces are cut off to expose end face holes of the membrane wires to form the membrane module 50, through holes 1042 are reserved through section cutting so as to be connected with the quick-screwing connector 1046 for air inlet, the test module can be conveniently replaced through a pull-plug design, then the middle unit 104 is hermetically connected with the upper unit 102 and the lower unit 106, the assembly of the module testing module 10 is realized, the membrane module 50 is convenient to disassemble and replace, the membrane wires 502 on the membrane module 50 are straightened as much as possible through the support rod 1048 to be evenly arranged, the measurement accuracy is ensured, and the quantitative comparison is facilitated. The pressure driving and the accurate regulation and control of the pressure are realized through the pressure driving and controlling module 20, the pressure is provided for the component testing module 10, the gas flow detecting module is a high-precision gas flowmeter, the measuring range of the high-precision gas flowmeter is 0-100ml/min, the permeation gas flow is detected through the gas flow detecting module under the control of various modes and parameters, the gas flow at the permeation side is accurately measured, data support is provided for the performance test of each gas-permeable membrane, and the quantitative detection of various membrane performances is favorably realized in the same device. The control system 40 is used for controlling the operation of the whole device, realizing the functions of pressure, test time setting, real-time curve monitoring and the like, and can be set into a constant pressure mode and a boosting mode, wherein the constant pressure mode is used for pre-detection, permeability coefficient test and integrity test, and the boosting mode is used for implosion pressure test.
The membrane module 50 may be a flat gas-permeable membrane, and is directly connected between the upper unit 102 and the lower unit 106 in a sealed manner.
Further, as shown in fig. 1, the upper unit 102 includes an upper cylinder 1022, an intake port 1024, a first exhaust port 1026, a first solenoid valve 1026, an intake side pressure sensor 1030, and the like. The gas inlet 1024 is disposed on the top surface of the upper cylinder 1022, and is connected to the pressure driving module through a pipeline, so that the pressure driving module can input gas to the component testing module 10 through the gas inlet 1024 to provide pressure. The first exhaust port 1026 is disposed on the side of the upper cylinder 1022, and a first electromagnetic valve 1026 is disposed on an exhaust pipeline connected to the upper cylinder, and is opened to exhaust air when the air in the exhaust device is exhausted and the exhaust pipeline is connected to an external gas collection and processing device to perform classification processing on different gases. An intake side pressure sensor 1030 is connected to the side of the upper cylinder 1022, and the height of the connection position on the upper cylinder 1022 is higher than the height of the first exhaust port 1026, and the intake side pressure sensor 1030 is in communication with the control system 40 for detecting the amount of intake pressure, so that the intake pressure of the control system 40 can be adjusted to reach the set test pressure.
In addition, a temperature sensor may be connected to the top surface of the upper barrel 1022, and the temperature sensor is in communication with the control system 40 to provide temperature data of the gas inside the upper barrel 1022.
Further, as shown in fig. 1, the lower unit 106 includes: a lower cylinder 1062, a second exhaust port 1064, a second solenoid valve 1066, and a gas-permeation-side pressure sensor 1068. The second exhaust port 1064 is disposed on the side of the lower cylinder 1062, the second exhaust port 1064 is connected to the gas flow rate detection module, and the exhaust pipe connected to the second exhaust port 1064 is provided with a second electromagnetic valve 1066, which is normally open during the test process, and is closed after the test is completed, so that the gas flow rate detection module 30 can detect the flow rate of the permeating gas, and the gas flow rate detection module 30 can be protected to some extent. The gas permeation side pressure sensor 1068 is connected to the side of the lower cylinder 1062, the height of the connection position on the lower cylinder 1062 is higher than that of the second exhaust port 1064, the gas permeation side pressure sensor 1068 is in communication connection with the control system 40 and is used for monitoring permeation side pressure, pre-inspection is performed at the initial operation stage of the device, whether the membrane module 50 is intact or not is preliminarily judged, whether the air tightness of the device is problem-free or not is judged, more accurate data can be obtained when later-stage testing is facilitated, and unnecessary testing errors are avoided.
Further, as shown in fig. 1 and 2, the upper unit 102, the middle unit 104, and the lower unit 106 are hermetically connected by threads and a sealing ring 108, and the upper end and the lower end of the middle unit 104 are respectively sleeved into the upper unit 102 and the lower unit 106, so that on one hand, the disassembly is convenient, on the other hand, the sealing performance is good, and the air tightness of the device is ensured. The middle unit 104 is provided with two through holes 1042 and two non-through holes 1044 which are distributed in a cross shape, the through holes 1042 are one-to-one arranged with the quick-screwing connectors 1046, and the non-through holes 1044 are one-to-one arranged with the connecting rods, so that the mounting and fixing stability of the membrane module 50 is further guaranteed, and the smooth proceeding of the test is further guaranteed.
Specifically, the through-hole 1042 may be an internally threaded through-hole 1042, and the non-through-hole 1044 may be an internally threaded non-through-hole 1044.
Further, the supporting rod 1048 is a telescopic adjustable supporting rod 1048, the length adjustment range of the telescopic adjustable supporting rod 1048 is 5cm-15cm, and the telescopic adjustable supporting rod 1048 can be adapted to various types of membrane assemblies 50, as shown in fig. 3, the supporting rod 1048 straightens the membrane filaments 502 in the membrane assemblies 50 downward, so that the membrane filaments are uniformly arranged, and a better test is facilitated.
Further, as shown in fig. 1, the pressure driving control module 20 includes: a plurality of high-pressure gas cylinders 202 that set up in parallel, respectively with component test module 10 tube coupling, for example can set up three high-pressure gas cylinders 202, be equipped with nitrogen gas, oxygen, carbon dioxide in each high-pressure gas cylinder 202 respectively, each sets up a relief pressure valve 204 on the gas outlet connecting line of each high-pressure gas cylinder 202 for gaseous outflow of control, set up electric proportional control valve 206 on the connecting line that is close to component test module 10, be used for accurate regulation gas pressure, thereby can provide accurate gas pressure for component test module 10 under control system 40's control.
The operation method of the breathable film performance test integrated device comprises the following steps:
s1, respectively installing two ends of the packaged membrane module on the module testing module, installing two ends of the membrane module on quick-screwing connectors of a middle unit of the module testing module, adjusting the height of a supporting rod, and straightening a separation membrane downwards to enable the separation membrane to be uniformly distributed;
s2, the middle unit is screwed and sealed with the upper unit and the lower unit, and the component testing module is sequentially connected with the pressure driving and controlling module, the air inlet side pressure sensor, the air outlet side pressure sensor and the air outlet pipeline;
s3, starting the control system, and after the control system normally operates, starting the specified high-pressure gas cylinder and the pressure reducing valve thereof, and adjusting the test pressure;
s4, setting a pre-detection pressure, a boosting time and a voltage stabilizing time in a constant-pressure mode, opening a first electromagnetic valve connected with the upper unit of the component testing module and a second electromagnetic valve connected with the lower unit of the component testing module, controlling boosting, fully discharging air in the device, and then closing the first electromagnetic valve;
s5, after pressure stabilization, the permeation side pressure is monitored through a gas permeation side pressure sensor, and if the permeation side pressure is monitored to be maintained in a specified pressure range for a specified duration, it is determined that the membrane module is intact and the device has no problem in air tightness;
specifically, for example, the specified time is 5min, the specified pressure range is 0-3Kpa, and approaches to 0, the second electromagnetic valve is opened, and the gas is not held down at the lower side, and directly flows out after being detected by the gas flowmeter. Namely after pressure stabilization, the monitored permeation side pressure approaches to 0 or fluctuates in a small pressure range for 5min, and the membrane module is considered to be intact and the air tightness of the device has no problem.
S6, after the pressure of the control device is relieved, the control device is adjusted to a constant pressure mode, the test pressure, the boosting time and the voltage stabilization test time are set, the boosting is controlled to be started, the ventilation coefficient test is carried out, the value range of the test pressure is 0.1MPa-0.3MPa, the value range of the boosting time is 5min-10min, and the voltage stabilization test time is not less than 30 min;
s7, detecting the flow of the permeating gas in real time through a gas flow detection module after the pressure is constant;
calculating the permeability coefficient according to the flow of the permeating gas and a preset formula, wherein the preset formula is as follows:
F=Q/(ΔP·S),
wherein F is characterized by an air permeability coefficient (mL cm)-2·min-1·bar-1) Q is characterized by the permeate gas flow (ml/min) and Δ P is characterized by the transmembrane pressure difference (bar), i.e. the set test pressure; s is characterized by the effective area of the membrane (cm)2);
S8, after the pressure of the control device is relieved, the control device is adjusted to a constant pressure mode, test pressure, pressure boosting time and pressure stabilizing test time are set, the nitrogen high-pressure gas cylinder is controlled to start boosting, and membrane integrity test is carried out, wherein the value range of the test pressure is 0.1-0.3 MPa, the value range of the pressure boosting time is 5-10 min, and the pressure stabilizing test time is not less than 30 min;
s9, after the pressure of the control device is relieved, the control device starts to boost the pressure by adopting an oxygen high-pressure gas cylinder under the same constant pressure mode, and after the pressure is constant, the gas flow detection module detects the flow of the oxygen permeating through the gas in real time;
s10, after the pressure of the control device is relieved, the control device starts and boosts the pressure by adopting a carbon dioxide high-pressure gas cylinder under the same constant pressure mode, and after the pressure is constant, the gas flow detection module detects the flow of the carbon dioxide gas permeating in real time;
s11, calculating the ratio of any two of the flow of the nitrogen gas, the flow of the oxygen gas and the flow of the carbon dioxide gas, wherein the ratio is determined by a larger value and a smaller value;
s12, if any ratio is far larger than 1, determining that the integrity of the membrane module is good, and if the ratio is close to 1, determining that the integrity of the membrane module has a problem;
specifically, for example, if the ratio is greater than 10, it is determined that the ratio is much greater than 1, the integrity of the membrane module is good, the ratio is 0.9-1.1, it is determined that the ratio approaches 1, the integrity of the membrane module has a problem,
s13, after the pressure of the control device is relieved, the control device is adjusted to a boosting mode, the maximum test pressure and boosting time are set, the boosting is controlled to start, and the implosion pressure test is carried out;
s14, in the boosting process, the flow of the permeated gas is detected in real time through the gas flow detection module, the test pressure is detected in real time through the gas inlet side pressure sensor, and a relation curve graph of the test pressure and the flow of the permeated gas is generated;
s15, if the increase value of the permeation gas flow in unit time is larger than the preset value, determining that the membrane is broken, stopping boosting, and determining that the maximum value of the test pressure corresponding to the permeation gas flow in unit time is the bursting pressure in the membrane;
specifically, for example, the unit time is set to 5s, the preset value is 5ml/min,
and S16, controlling to save data, reset pressure, remove components and turn off power supply after the test is finished.
The operation method of the integrated device for testing the performance of the breathable film realizes the detection of the air permeability coefficient, the integrity of the film and the burst pressure in the film, and quantifies the air permeability coefficient, the integrity of the film and the burst pressure in the film, thereby facilitating the comparison of the product performance. After the membrane assembly is installed for one time, the tests of three performance parameters of the air permeability coefficient, the membrane integrity and the intra-membrane burst pressure can be sequentially realized, so that the test efficiency is greatly improved.
In addition, after the pressure of the control device is relieved, if gas needs to be replaced, the first electromagnetic valve of the upper unit of the component testing module is opened, original gas is exhausted through boosting, then the first electromagnetic valve is closed, and the next program is started, so that the detection accuracy can be further improved.
The integrated device for testing the performance of the breathable film and the operation method thereof can quickly and accurately test the burst pressure in the separation film, and can comprehensively evaluate the breathable performance and the integrity of the separation film, thereby realizing the real multiple purposes of one machine; the device has the real-time on-line monitoring function of numerical values, the data feedback is timely, and the measurement accuracy is high; the test operation method has important significance for the perfection of the current domestic breathable film performance evaluation method, and the device has the advantages of attractive appearance, convenience in disassembly, simplicity and practicability in operation method, and is suitable for the research and application of the hollow fiber breathable film technology.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. The utility model provides a ventilated membrane capability test integrated device which characterized in that includes:
the subassembly test module, with the pressure drive control module of the top tube coupling of subassembly test module, with the gas flow detection module that the bottom of subassembly test module is connected, respectively with the subassembly test module the pressure drive control module and the control system that the gas flow detection module communication is connected, the subassembly test module includes:
the upper unit, the middle unit and the lower unit are sequentially connected in a sealing manner from top to bottom, and the upper unit is connected with the pressure driving module through a pipeline; the middle unit is provided with a through hole and a non-through hole from bottom to top, the bottom end of the through hole is detachably connected with a quick-screwing joint, the bottom end of the quick-screwing joint is detachably connected with a membrane assembly, and the bottom end of the non-through hole is detachably connected with a support rod.
2. The integrated device for testing the performance of the breathable film according to claim 1,
the upper unit includes: an upper cylinder body; the air inlet is arranged on the top surface of the upper cylinder body and is connected with the pressure driving module through a pipeline; a first exhaust port arranged on the side surface of the upper cylinder body, and an exhaust pipeline connected with the first exhaust port is provided with a first electromagnetic valve; and the air inlet side pressure sensor is connected to the side surface of the upper barrel, the height of the connecting position of the air inlet side pressure sensor on the upper barrel is higher than that of the first exhaust port, and the air inlet side pressure sensor is in communication connection with the control system.
3. The integrated device for testing the performance of the breathable film according to claim 1,
the lower unit includes: a lower cylinder body; the second exhaust port is arranged on the side face of the lower cylinder body and is connected with the gas flow detection module through a pipeline, and a second electromagnetic valve is arranged on an exhaust pipeline connected with the second exhaust port; and the gas permeation side pressure sensor is connected to the side surface of the lower cylinder body, the height of the connection position of the gas permeation side pressure sensor on the lower cylinder body is higher than that of the second exhaust port, and the gas permeation side pressure sensor is in communication connection with the control system.
4. The integrated breathable film performance test device of any one of claims 1 to 4, wherein,
the upper unit, the middle unit and the lower unit are hermetically connected through threads and sealing rings, and the upper end and the lower end of the middle unit are sleeved in the upper unit and the lower unit respectively;
the middle unit is provided with two through holes and two non-through holes which are distributed in a crossed manner, the through holes and the non-through holes are arranged in a cross manner, the through holes and the quick-screwing joints are arranged in a one-to-one manner, and the non-through holes and the connecting rods are arranged in a one-to-one manner.
5. The integrated breathable film performance test device of any one of claims 1 to 4, wherein,
the support rod is a telescopic adjusting support rod, and the length adjusting range of the telescopic adjusting support rod is 5cm-15 cm; the gas flow detection module is a high-precision gas flowmeter, and the measuring range of the high-precision gas flowmeter is 0-100 ml/min.
6. The integrated breathable film performance test device of any one of claims 1 to 4, wherein,
the pressure driving and controlling module comprises: the device comprises a plurality of high-pressure gas cylinders which are arranged in parallel and are respectively connected with the component testing module through pipelines, a pressure reducing valve is respectively arranged on a gas outlet connecting pipeline of each high-pressure gas cylinder, and an electrical proportion regulating valve is arranged on a connecting pipeline close to the component testing module.
7. An operation method of the integrated device for testing the performance of the breathable film according to any one of claims 1 to 6, characterized by comprising the following steps:
installing two ends of the membrane assembly on quick-screwing connectors of a middle unit of the assembly testing module, adjusting the height of the supporting rod, and straightening the separation membrane downwards to enable the separation membrane to be uniformly distributed;
the middle unit is screwed and hermetically connected with the upper unit and the lower unit, and the component testing module is sequentially connected with the pressure driving and controlling module, the air inlet side pressure sensor, the air outlet side pressure sensor and the air outlet pipeline;
starting a control system, and after the control system normally operates, starting a specified high-pressure gas cylinder and a pressure reducing valve thereof, and adjusting the test pressure;
in a constant pressure mode, setting a pre-detection pressure, a boosting time and a voltage stabilizing time, opening a first electromagnetic valve connected with the upper unit of the component testing module and a second electromagnetic valve connected with the lower unit of the component testing module, controlling boosting, fully discharging air in the device, and then closing the first electromagnetic valve;
after the pressure is stabilized, monitoring the permeation side pressure through a gas permeation side pressure sensor, and if the monitored permeation side pressure is maintained in a specified pressure range for a specified time, determining that the membrane assembly is intact and the air tightness of the device has no problem;
after the pressure of the control device is relieved, carrying out an air permeability coefficient test or a membrane assembly integrity test or an implosion pressure test or carrying out the air permeability coefficient test and the membrane assembly integrity test in sequence or carrying out the air permeability coefficient test and the implosion pressure test in sequence or carrying out the air permeability coefficient test, the membrane assembly integrity test and the implosion pressure test in sequence;
and after the test is finished, controlling and storing data, resetting pressure, dismounting the assembly and turning off a power supply.
8. The operation method of the integrated device for testing the breathable film performance of claim 7, wherein the air permeability test comprises the following steps:
under a constant pressure mode, setting test pressure, boosting time and voltage stabilization test time, and controlling to start boosting, wherein the value range of the test pressure is 0.1-0.3 MPa, the value range of the boosting time is 5-10 min, and the voltage stabilization test time is not less than 30 min;
when the pressure is constant, detecting the flow of the permeating gas in real time through a gas flow detection module;
calculating the permeability coefficient according to the flow of the permeating gas and a preset formula, wherein the preset formula is as follows:
F=Q/(ΔP·S),
wherein F is characterized by an air permeability coefficient (mL cm)-2·min-1·bar-1) Q is characterized by the permeate gas flow (ml/min) and Δ P is characterized by the transmembrane pressure difference (bar), i.e. the set test pressure; s is characterized by the effective area of the membrane (cm)2)。
9. The operation method of the integrated device for testing the performance of the breathable film according to claim 7, wherein the film assembly integrity test comprises the following steps:
under a constant pressure mode, setting test pressure, boosting time and pressure stabilization test time, and controlling a nitrogen high-pressure gas cylinder to start boosting, wherein the value range of the test pressure is 0.1-0.3 MPa, the value range of the boosting time is 5-10 min, and the pressure stabilization test time is not less than 30 min;
when the pressure is constant, detecting the flow of the gas penetrating through the nitrogen in real time through a gas flow detection module;
after the pressure of the control device is relieved, an oxygen high-pressure gas cylinder is controlled to start boosting in the same constant pressure mode, and after the pressure is constant, the flow of the gas penetrating through the oxygen is detected in real time through a gas flow detection module;
after the pressure of the control device is relieved, a carbon dioxide high-pressure gas cylinder is controlled to start boosting in the same constant pressure mode, and after the pressure is constant, the flow of the carbon dioxide gas passing through is detected in real time by a gas flow detection module;
calculating the ratio of any two of the flow of the gas penetrating through the nitrogen, the flow of the gas penetrating through the oxygen and the flow of the gas penetrating through the carbon dioxide, wherein the ratio is determined by a larger value and a smaller value;
if any ratio is far larger than 1, the integrity of the membrane component is determined to be good;
if there is a ratio approaching 1, then it is determined that there is a problem with the integrity of the membrane module.
10. The operation method of the integrated device for testing the performance of the breathable film according to claim 7, wherein the internal burst pressure test comprises the following steps:
in the boosting mode, the maximum test pressure and the boosting time are set, and the starting and boosting are controlled;
in the boosting process, the flow of the permeated gas is detected in real time through a gas flow detection module, the test pressure is detected in real time through a pressure sensor at the gas inlet side, and a relation curve graph of the test pressure and the flow of the permeated gas is generated;
if the increase value of the flow rate of the permeating gas in unit time is larger than the preset value, the rupture of the membrane is determined, the pressure rise is stopped, and the maximum value of the test pressure corresponding to the flow rate of the permeating gas in unit time is determined as the bursting pressure in the membrane.
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